dataset_id
large_stringclasses
414 values
reaction_id
large_stringlengths
36
36
reaction_smiles
large_stringlengths
4
873
rxn_insight_reaction
large_stringlengths
19
1.07k
mapped_reaction_smiles
large_stringlengths
14
3.37k
reactant_smiles
large_stringlengths
1
581
product_smiles
large_stringlengths
1
433
reagent_smiles
large_stringclasses
634 values
catalyst_smiles
large_stringlengths
1
683
solvent_smiles
large_stringlengths
1
245
rxn_insight_class
large_stringclasses
11 values
rxn_insight_name
large_stringclasses
346 values
rxn_insight_tag
large_stringlengths
64
64
rxn_insight_tag2
large_stringlengths
64
64
rxn_insight_scaffold
large_stringlengths
5
288
rxn_insight_template
large_stringlengths
24
2.64k
yield_percent
float64
-0.8
90,205,160,000B
yield_measurements
large_stringlengths
2
864
temperature_value
float64
-230
30.1k
temperature_units
large_stringclasses
3 values
reaction_time_value
float64
0
4k
time_units
large_stringclasses
4 values
procedure_details
large_stringlengths
1
23.6k
reference
large_stringclasses
96 values
doi
large_stringclasses
19 values
functional_groups_reactants
large_stringlengths
3
716
functional_groups_products
large_stringlengths
3
539
participating_rings_reactants
large_stringlengths
5
293
participating_rings_products
large_stringlengths
5
271
all_rings_products
large_stringlengths
5
271
byproduct_smiles
large_stringclasses
176 values
agent_smiles
large_stringlengths
1
712
temperature_c
float64
-230
30.1k
reaction_time_hours
float64
0
2.16k
reaction_smiles_with_agents
large_stringlengths
4
882
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-909429328f9c43f0b3f4f7598de5461c
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(NC(=O)OC(C)(C)C)C(=O)OC)cc1>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(N)C(=O)OC)cc1
C(C)(C)(C)OC(=O)NC(C(=O)OC)CC1=CC=C(C=C1)OCCN1C(SC2=C1C=CC(=C2)C(C2=CC=CC=C2)=NOC)=O.C(=O)(C(F)(F)F)O>>NC(C(=O)OC)CC1=CC=C(C=C1)OCCN1C(SC2=C1C=CC(=C2)C(C2=CC=CC=C2)=NOC)=O
CC(C)(C)OC(=O)[NH:30][CH:29]([CH2:28][c:27]1[cH:26][cH:25][c:24]([O:23][CH2:22][CH2:21][n:20]2[c:14]3[cH:13][cH:12][c:11]([C:4](=[N:3][O:2][CH3:1])[c:5]4[cH:6][cH:7][cH:8][cH:9][cH:10]4)[cH:16][c:15]3[s:17][c:18]2=[O:19])[cH:36][cH:35]1)[C:31](=[O:32])[O:33][CH3:34]>>[CH3:1][O:2][N:3]=[C:4]([c:5]1[cH:6][cH:7][cH:8][cH:...
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(NC(=O)OC(C)(C)C)C(=O)OC)cc1
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(N)C(=O)OC)cc1
null
null
C(Cl)Cl
Reduction
Hydrogenolysis of amides/imides/carbamates
3c33dd2a2d355ee5ba0287367e209aa147a39aa00607f0c95fb2bf1ade45d014
c5b5dffe7dd8beebdc1baa8b5b05300a9f7079e65dcfd42ade6f8a77ff09537d
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
C-C(-C)(-C)-O-C(=O)-[NH;D2;+0:1]-[C:2](-[C:3])-[C:4](=[O;D1;H0:5])-[#8:6]-[C;D1;H3:7]>>[C:3]-[C:2](-[NH2;D1;+0:1])-[C:4](=[O;D1;H0:5])-[#8:6]-[C;D1;H3:7]
null
[]
null
null
5
HOUR
Dissolve the compound obtained in Example 10 (1 eq.) in 250 ml of anhydrous DCM and add TFA (20 eq.) dropwise. Stir for 5 hours and evaporate. Take up in water and render alkaline using 10% K2CO3. Extract with ethyl acetate. Wash the organic phases with water, dry over MgSO4, filter and evaporate. Take up in a minimum ...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Primary amine
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
C(Cl)Cl
null
5
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(NC(=O)OC(C)(C)C)C(=O)OC)cc1>C(Cl)Cl>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(N)C(=O)OC)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-860dedf2fc534956b98b8e133ac89c91
CI.COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)NC(=O)OC(C)(C)C>>COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)N(C)C(=O)OC(C)(C)C
Cl.C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)OC)NC(=O)OC(C)(C)C)C=C1.CI.[H-].[Na+]>>C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)OC)N(C)C(=O)OC(C)(C)C)C=C1
I[CH3:35].[CH3:1][O:2][C:3](=[O:4])[CH:5]([CH2:6][c:7]1[cH:8][cH:9][c:10]([O:11][CH2:12][CH2:13][n:14]2[c:15](=[O:16])[s:17][c:18]3[cH:19][c:20]([C:21](=[O:22])[c:23]4[cH:24][cH:25][cH:26][cH:27][cH:28]4)[cH:29][cH:30][c:31]23)[cH:32][cH:33]1)[NH:34][C:36](=[O:37])[O:38][C:39]([CH3:40])([CH3:41])[CH3:42]>>[CH3:1][O:2][...
CI.COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)NC(=O)OC(C)(C)C
COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)N(C)C(=O)OC(C)(C)C
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
29c841ae076cb6ee785aad2a4e3ce1a9b47357d7ad25657b8d9991b1347f5721
c485eddcb40c5a0d396ffdb624041effa09ee4f5ca2ecce3fe13077cf65004ed
O=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
I-[CH3;D1;+0:1].[C:2]-[C:3](-[NH;D2;+0:4]-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3:11])-[C:12](=[O;D1;H0:13])-[#8:14]-[C;D1;H3:15]>>[C:2]-[C:3](-[C:12](=[O;D1;H0:13])-[#8:14]-[C;D1;H3:15])-[N;H0;D3;+0:4](-[CH3;D1;+0:1])-[C:5](=[O;D1;H0:6])-[#8:7]-[C:8](-[C;D1;H3:9])(-[C;D1;H3:10])-[C;D1;H3...
null
[]
null
null
null
null
Dissolve the compound obtained in Step C of Example 10 (1 eq.) and CH3I (2 eq.): in 55 ml of anhydrous DMF and place in an ice bath at 0° C. Add NaH (1.5 eq.) in portions. Allow to return to ambient temperature. Hydrolyse, acidify with 1N HCl and filter. Purify the resulting crude product by chromatography on silica ge...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester
Carbamic ester
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HI
CN(C)C=O
null
null
CI.COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)NC(=O)OC(C)(C)C>CN(C)C=O>COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)N(C)C(=O)OC(C)(C)C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-708b24f2e5e34bcf94303c04d4f13d44
COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)N(C)C(=O)OC(C)(C)C.CON>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(C(=O)OC)N(C)C(=O)OC(C)(C)C)cc1
C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)OC)N(C)C(=O)OC(C)(C)C)C=C1.CON>>C(C)(C)(C)OC(=O)N(C(C(=O)OC)CC1=CC=C(C=C1)OCCN1C(SC2=C1C=CC(=C2)C(C2=CC=CC=C2)=NOC)=O)C
O=[C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[c:11]1[cH:12][cH:13][c:14]2[c:15]([cH:16]1)[s:17][c:18](=[O:19])[n:20]2[CH2:21][CH2:22][O:23][c:24]1[cH:25][cH:26][c:27]([CH2:28][CH:29]([C:30](=[O:31])[O:32][CH3:33])[N:34]([CH3:35])[C:36](=[O:37])[O:38][C:39]([CH3:40])([CH3:41])[CH3:42])[cH:43][cH:44]1.[CH3:1][O:2][NH2:...
COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)N(C)C(=O)OC(C)(C)C.CON
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(C(=O)OC)N(C)C(=O)OC(C)(C)C)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step A, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-methylhydroxylamine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
null
null
null
COC(=O)C(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)N(C)C(=O)OC(C)(C)C.CON>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(C(=O)OC)N(C)C(=O)OC(C)(C)C)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-11eebd30777b45dc9263fedb0c3509d0
CON.O=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1
C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC2C(OC3=C2C=CC=C3)=O)C=C1.CON>>CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC2C(OC3=C2C=CC=C3)=O)C=C1)C1=CC=CC=C1
[CH3:1][O:2][NH2:3].O=[C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[c:11]1[cH:12][cH:13][c:14]2[c:15]([cH:16]1)[s:17][c:18](=[O:19])[n:20]2[CH2:21][CH2:22][O:23][c:24]1[cH:25][cH:26][c:27]([CH2:28][CH:29]2[C:30](=[O:31])[O:32][c:33]3[cH:34][cH:35][cH:36][cH:37][c:38]32)[cH:39][cH:40]1>>[CH3:1][O:2][N:3]=[C:4]([c:5]1[cH...
CON.O=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step A, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-methylhydroxylamine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1.c1ccc2c(c1)CCO2
HO-
null
null
null
CON.O=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c1cef0531c944d71b832c83ba61f51c7
CO.CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(C(=O)OC)c2ccccc2O)cc1
CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC2C(OC3=C2C=CC=C3)=O)C=C1)C1=CC=CC=C1.CO>>OC1=C(C=CC=C1)C(C(=O)OC)CC1=CC=C(C=C1)OCCN1C(SC2=C1C=CC(=C2)C(C2=CC=CC=C2)=NOC)=O
[OH:32][CH3:33].[CH3:1][O:2][N:3]=[C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[c:11]1[cH:12][cH:13][c:14]2[c:15]([cH:16]1)[s:17][c:18](=[O:19])[n:20]2[CH2:21][CH2:22][O:23][c:24]1[cH:25][cH:26][c:27]([CH2:28][CH:29]2[C:30](=[O:31])[O:40][c:39]3[c:34]2[cH:35][cH:36][cH:37][cH:38]3)[cH:41][cH:42]1>>[CH3:1][O:2][N:3]=[C:...
CO.CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(C(=O)OC)c2ccccc2O)cc1
null
null
S(O)(O)(=O)=O
Protection
OtherReaction
6cfd4d1df6f9006d5687793df661d40f989ff8374937b623a149a85c7a294a6a
5e4632d88056171b71c6999a966b3ed8f4e96271d8ecc461eaaa15cb46640ba7
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CCc2ccccc2)cc1
[C;D1;H3:1]-[OH;D1;+0:2].[C:3]-[C:4]1-[c:5]:[c:6](:[c:7])-[O;H0;D2;+0:8]-[C;H0;D3;+0:9]-1=[O;D1;H0:10]>>[C:3]-[C:4](-[c:5]:[c:6](-[OH;D1;+0:8]):[c:7])-[C;H0;D3;+0:9](=[O;D1;H0:10])-[O;H0;D2;+0:2]-[C;D1;H3:1]
null
[]
null
null
null
null
1.5 g of the compound obtained in Step B, in 50 ml of methanol and 0.1 ml of concentrated sulphuric acid, are heated at reflux for 2 hours. The solvent is then evaporated off, the residue is hydrolysed and the precipitate obtained is chromatographed on silica gel (eluant: AcOEt/toluene 5/95). Conditions: See reaction.n...
10.6084/m9.figshare.5104873.v1
null
Ester.Methanol
Ester.Aromatic alcohol
c1ccc2c(c1)CCO2
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1.c1ccccc1
null
S(O)(O)(=O)=O
null
null
CO.CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC2C(=O)Oc3ccccc32)cc1>S(O)(O)(=O)=O>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(C(=O)OC)c2ccccc2O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-79a3ed52a681452f9e6408051ec6d478
COC(=O)C(Cc1ccccc1)Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(Cc2ccccc2)C(=O)OC)cc1
C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(CC(C(=O)OC)CC3=CC=CC=C3)C=C2)C=C1.CON>>C(C1=CC=CC=C1)C(C(=O)OC)CC1=CC=C(C=C1)OCCN1C(SC2=C1C=CC(=C2)C(C2=CC=CC=C2)=NOC)=O
O=[C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[c:11]1[cH:12][cH:13][c:14]2[c:15]([cH:16]1)[s:17][c:18](=[O:19])[n:20]2[CH2:21][CH2:22][O:23][c:24]1[cH:25][cH:26][c:27]([CH2:28][CH:29]([CH2:30][c:31]2[cH:32][cH:33][cH:34][cH:35][cH:36]2)[C:37](=[O:38])[O:39][CH3:40])[cH:41][cH:42]1.[CH3:1][O:2][NH2:3]>>[CH3:1][O:2][N:3...
COC(=O)C(Cc1ccccc1)Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(Cc2ccccc2)C(=O)OC)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CCCc2ccccc2)cc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step A, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-methylhydroxylamine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1.c1ccccc1
HO-
null
null
null
COC(=O)C(Cc1ccccc1)Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(Cc2ccccc2)C(=O)OC)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b3e19273d94248e8a46697073c36fcfe
COC(=O)C(CCc1ccccc1)Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(CCc2ccccc2)C(=O)OC)cc1
C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(CC(C(=O)OC)CCC3=CC=CC=C3)C=C2)C=C1.CON>>CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(CC(C(=O)OC)CCC3=CC=CC=C3)C=C2)C=C1)C1=CC=CC=C1
O=[C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[c:11]1[cH:12][cH:13][c:14]2[c:15]([cH:16]1)[s:17][c:18](=[O:19])[n:20]2[CH2:21][CH2:22][O:23][c:24]1[cH:25][cH:26][c:27]([CH2:28][CH:29]([CH2:30][CH2:31][c:32]2[cH:33][cH:34][cH:35][cH:36][cH:37]2)[C:38](=[O:39])[O:40][CH3:41])[cH:42][cH:43]1.[CH3:1][O:2][NH2:3]>>[CH3:1][...
COC(=O)C(CCc1ccccc1)Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(CCc2ccccc2)C(=O)OC)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CCCCc2ccccc2)cc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step A, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-methylhydroxylamine. The two (Z) and (E) compounds are not separated. Conditions: See reaction.notes.procedure_details. Workup: The two (Z) and (E) compounds are not separated
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1.c1ccccc1
HO-
null
null
null
COC(=O)C(CCc1ccccc1)Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(CCc2ccccc2)C(=O)OC)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-eee1c52aaa5b4766814cbe2cf60d8cf5
CCOC(=O)C(C)(C)Oc1ccc(OCCCl)cc1.O=C(c1ccccc1)c1ccc2c(c1)S(=O)C=N2>>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1
[OH-].[Na+].C(C1=CC=CC=C1)(=O)C1=CC2=C(N=CS2=O)C=C1.C(=O)([O-])[O-].[K+].[K+].ClCCOC1=CC=C(OC(C(=O)OCC)(C)C)C=C1>>C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1
Cl[CH2:16][CH2:15][O:14][c:13]1[cH:12][cH:11][c:10]([O:9][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH3:8])[cH:36][cH:35]1.[N:17]1=[CH:18][S:20](=[O:19])[c:21]2[cH:22][c:23]([C:24](=[O:25])[c:26]3[cH:27][cH:28][cH:29][cH:30][cH:31]3)[cH:32][cH:33][c:34]21>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH3:8])[O...
CCOC(=O)C(C)(C)Oc1ccc(OCCCl)cc1.O=C(c1ccccc1)c1ccc2c(c1)S(=O)C=N2
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1
null
null
O.CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
42c83f048334b1ed148ed7afdbd743f45dba21a36b3061112c38545e7e60436d
3dcb031a7507da808ae5e1b8f13ca2c4f0152648164857a941ec9d83076e2a56
O=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
Cl-[CH2;D2;+0:1]-[C:2]-[#8:3].[O;H0;D1;+0:4]=[S;H0;D3;+0:5]1-[CH;D2;+0:6]=[N;H0;D2;+0:7]-[c:8](:[c:9]):[c:10]-1:[c:11]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:7]1:[c:8](:[c:9]):[c:10](:[c:11]):[s;H0;D2;+0:5]:[c;H0;D3;+0:6]:1=[O;H0;D1;+0:4]
null
[]
120
CELSIUS
null
null
To a solution, heated at 80° C. for 2 hours, of 6-benzoyl-benzothiazolinone (6.7 mmol) in the presence of K2CO3 in 20 ml of DMF there is added ethyl 2-[4-(2-chloroethoxy)phenoxy]-2-methylpropanoate. The reaction mixture is heated at 120° C. for 5 days, cooled, hydrolysed using 100 ml of water and rendered alkaline usin...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Sulfoxide
null
c1ccc2scnc2c1
c1ccc2scnc2c1
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HCl
O.CN(C)C=O
120
null
CCOC(=O)C(C)(C)Oc1ccc(OCCCl)cc1.O=C(c1ccccc1)c1ccc2c(c1)S(=O)C=N2>O.CN(C)C=O>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b5f77654d99d40ec94ce5c7a18edac57
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
Cl.C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1.Cl.CON>>CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1)C1=CC=CC=C1
O=[C:24]([c:23]1[cH:22][c:21]2[s:20][c:18](=[O:19])[n:17]([CH2:16][CH2:15][O:14][c:13]3[cH:12][cH:11][c:10]([O:9][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH3:8])[cH:38][cH:37]3)[c:36]2[cH:35][cH:34]1)[c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1.[NH2:25][O:26][CH3:27]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7...
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
null
null
N1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
A solution of the compound obtained in Step A (500 mg) and O-methylhydroxylamine hydrochloride (165 mg) in 15 ml of pyridine is heated at reflux for 3 hours. The reaction mixture is hydrolysed using 100 ml of ice-cold water, acidified using 6N HCl and then extracted with ethyl acetate. The organic phase is dried over m...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
N1=CC=CC=C1
null
null
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>N1=CC=CC=C1>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f46bba6eaa754bbfac2c0e0b61e99bc0
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.NO>>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1
Cl.C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1.Cl.NO>>ON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1)C1=CC=CC=C1
O=[C:24]([c:23]1[cH:22][c:21]2[s:20][c:18](=[O:19])[n:17]([CH2:16][CH2:15][O:14][c:13]3[cH:12][cH:11][c:10]([O:9][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH3:8])[cH:37][cH:36]3)[c:35]2[cH:34][cH:33]1)[c:27]1[cH:28][cH:29][cH:30][cH:31][cH:32]1.[NH2:25][OH:26]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH3...
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.NO
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1
null
null
N1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
b5fd91d879f097d0ef2e8e2d3ef7d2ef0195968870a9602a47b8324c601790b9
1a0ef15294bdb221fb8888b5d4c7fcf00473b11e53da288791d32747daa48d23
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[NH2;D1;+0:10]-[O;D1;H1:11]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:10]-[O;D1;H1:11])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
A solution of the compound obtained in Step A of Example 31 (500 mg) and hydroxylamine hydrochloride (137 mg) in 10 ml of pyridine is heated at reflux for 3 hours. The reaction mixture is hydrolysed using 100 ml of ice-cold water and is acidified using 6N HCl. The precipitate obtained is then filtered off, washed with ...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
Oxime
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
N1=CC=CC=C1
null
null
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.NO>N1=CC=CC=C1>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-264340a5610d49d1950476b864cc05dc
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1>>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(OC(C)(C)C(=O)O)cc1
Cl.CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1)C1=CC=CC=C1.[OH-].[K+]>>CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)O)(C)C)C=C2)C=C1)C1=CC=CC=C1
CC[O:34][C:32]([C:29]([O:28][c:27]1[cH:26][cH:25][c:24]([O:23][CH2:22][CH2:21][n:20]2[c:14]3[cH:13][cH:12][c:11]([C:4](=[N:3][O:2][CH3:1])[c:5]4[cH:6][cH:7][cH:8][cH:9][cH:10]4)[cH:16][c:15]3[s:17][c:18]2=[O:19])[cH:36][cH:35]1)([CH3:30])[CH3:31])=[O:33]>>[CH3:1][O:2][N:3]=[C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[...
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(OC(C)(C)C(=O)O)cc1
null
null
C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
To a solution of the compound obtained in Step B of Example 31 (0.8 g) in 5 ml of ethanol 95° there is added potassium hydroxide (100 mg) dissolved in 1 ml of ethanol 95° The reaction mixture is heated at reflux overnight. After cooling to ambient temperature, the solution is acidified using 1N HCl. The precipitate obt...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
Other
C(C)O
null
null
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1>C(C)O>CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(OC(C)(C)C(=O)O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5476e58a4d654c8d9d6fe2c2dbb09b99
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1>>CC(C)(Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1)C(=O)O
Cl.ON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1)C1=CC=CC=C1.[OH-].[K+]>>ON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)O)(C)C)C=C2)C=C1)C1=CC=CC=C1
CC[O:35][C:33]([C:2]([CH3:1])([CH3:3])[O:4][c:5]1[cH:6][cH:7][c:8]([O:9][CH2:10][CH2:11][n:12]2[c:13](=[O:14])[s:15][c:16]3[cH:17][c:18]([C:19](=[N:20][OH:21])[c:22]4[cH:23][cH:24][cH:25][cH:26][cH:27]4)[cH:28][cH:29][c:30]23)[cH:31][cH:32]1)=[O:34]>>[CH3:1][C:2]([CH3:3])([O:4][c:5]1[cH:6][cH:7][c:8]([O:9][CH2:10][CH2:...
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1
CC(C)(Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1)C(=O)O
null
null
C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
To a solution of the compound obtained in Example 32 (0.5 g) in 5 ml of ethanol 95° there is added potassium hydroxide (107 mg) dissolved in 1 ml of ethanol 95°. The reaction mixture is heated at reflux overnight. After cooling to ambient temperature, the solution is acidified using 1N HCl. The precipitate obtained is ...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
Other
C(C)O
null
null
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1>C(C)O>CC(C)(Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4ccccc4)ccc32)cc1)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-82f2de4777404c1f83fd80eb7ede4828
CCOC(=O)C(C)(C)Oc1ccc(OCCCl)cc1.O=C(c1cccc(Cl)c1)c1ccc2c(c1)S(=O)C=N2>>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1
[OH-].[Na+].ClC=1C=C(C(=O)C2=CC3=C(N=CS3=O)C=C2)C=CC1.C(=O)([O-])[O-].[K+].[K+].ClCCOC1=CC=C(OC(C(=O)OCC)(C)C)C=C1>>ClC=1C=C(C(=O)C2=CC3=C(N(C(S3)=O)CCOC3=CC=C(OC(C(=O)OCC)(C)C)C=C3)C=C2)C=CC1
Cl[CH2:16][CH2:15][O:14][c:13]1[cH:12][cH:11][c:10]([O:9][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH3:8])[cH:37][cH:36]1.[N:17]1=[CH:18][S:20](=[O:19])[c:21]2[cH:22][c:23]([C:24](=[O:25])[c:26]3[cH:27][cH:28][cH:29][c:30]([Cl:31])[cH:32]3)[cH:33][cH:34][c:35]21>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([C...
CCOC(=O)C(C)(C)Oc1ccc(OCCCl)cc1.O=C(c1cccc(Cl)c1)c1ccc2c(c1)S(=O)C=N2
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1
null
null
O.CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
42c83f048334b1ed148ed7afdbd743f45dba21a36b3061112c38545e7e60436d
3dcb031a7507da808ae5e1b8f13ca2c4f0152648164857a941ec9d83076e2a56
O=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
Cl-[CH2;D2;+0:1]-[C:2]-[#8:3].[O;H0;D1;+0:4]=[S;H0;D3;+0:5]1-[CH;D2;+0:6]=[N;H0;D2;+0:7]-[c:8](:[c:9]):[c:10]-1:[c:11]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:7]1:[c:8](:[c:9]):[c:10](:[c:11]):[s;H0;D2;+0:5]:[c;H0;D3;+0:6]:1=[O;H0;D1;+0:4]
null
[]
120
CELSIUS
null
null
To a solution, heated at 80° C. for 2 hours, of 6-(3′-chlorobenzoyl)-benzothiazolinone (1.8 g) in the presence of K2CO3 (1.72 g) in 20 ml of DMF there is added ethyl 2-[4-(2-chloroethoxy)phenoxy]-2-methylpropanoate (1.96 g). The reaction mixture is heated at 120° C. for 5 days, cooled, hydrolysed using 100 ml of water ...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Sulfoxide
null
c1ccc2scnc2c1
c1ccc2scnc2c1
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HCl
O.CN(C)C=O
120
null
CCOC(=O)C(C)(C)Oc1ccc(OCCCl)cc1.O=C(c1cccc(Cl)c1)c1ccc2c(c1)S(=O)C=N2>O.CN(C)C=O>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-43e233c2fe6e4d73b14262eec7767f6c
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1.CON>>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4cccc(Cl)c4)ccc32)cc1
Cl.ClC=1C=C(C(=O)C2=CC3=C(N(C(S3)=O)CCOC3=CC=C(OC(C(=O)OCC)(C)C)C=C3)C=C2)C=CC1.Cl.CON>>ClC=1C=C(C=CC1)C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1)=NOC
O=[C:24]([c:23]1[cH:22][c:21]2[s:20][c:18](=[O:19])[n:17]([CH2:16][CH2:15][O:14][c:13]3[cH:12][cH:11][c:10]([O:9][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH3:8])[cH:39][cH:38]3)[c:37]2[cH:36][cH:35]1)[c:28]1[cH:29][cH:30][cH:31][c:32]([Cl:33])[cH:34]1.[NH2:25][O:26][CH3:27]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6...
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1.CON
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4cccc(Cl)c4)ccc32)cc1
null
null
N1=CC=CC=C1
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
A solution of the compound obtained in Step A (1.00 g) and O-methylhydroxylamine hydrochloride (309 mg) in 15 ml of pyridine is heated at reflux for 3 hours. The reaction mixture is hydrolysed using 100 ml of ice-cold water and acidified using 6N HCl. The precipitate obtained is filtered off, washed with water and then...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
N1=CC=CC=C1
null
null
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1.CON>N1=CC=CC=C1>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4cccc(Cl)c4)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b14af2bb85a04671a97996f852d4bdb4
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4cccc(Cl)c4)ccc32)cc1>>CC(C)(Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4cccc(Cl)c4)ccc32)cc1)C(=O)O
Cl.ClC=1C=C(C=CC1)C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1)=NO.[OH-].[K+]>>ClC=1C=C(C=CC1)C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)O)(C)C)C=C2)C=C1)=NO
CC[O:36][C:34]([C:2]([CH3:1])([CH3:3])[O:4][c:5]1[cH:6][cH:7][c:8]([O:9][CH2:10][CH2:11][n:12]2[c:13](=[O:14])[s:15][c:16]3[cH:17][c:18]([C:19](=[N:20][OH:21])[c:22]4[cH:23][cH:24][cH:25][c:26]([Cl:27])[cH:28]4)[cH:29][cH:30][c:31]23)[cH:32][cH:33]1)=[O:35]>>[CH3:1][C:2]([CH3:3])([O:4][c:5]1[cH:6][cH:7][c:8]([O:9][CH2:...
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4cccc(Cl)c4)ccc32)cc1
CC(C)(Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4cccc(Cl)c4)ccc32)cc1)C(=O)O
null
null
C(C)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
To a solution of the compound obtained in Example 37 (0.6 g) in 5 ml of ethanol 95° there is added potassium hydroxide (90 mg) dissolved in 1 ml of ethanol 95°. The reaction mixture is heated at reflux overnight. After cooling to ambient temperature, the solution is acidified using 1N HCl. The precipitate obtained is t...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
Other
C(C)O
null
null
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4cccc(Cl)c4)ccc32)cc1>C(C)O>CC(C)(Oc1ccc(OCCn2c(=O)sc3cc(C(=NO)c4cccc(Cl)c4)ccc32)cc1)C(=O)O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a075e7720b934c6fb85c6f4b2e0ba3cb
CCOC(=O)C(C)(C)CCCOc1ccc(OCCCl)cc1.O=C(c1ccccc1)c1ccc2c(c1)S(=O)C=N2>>CCOC(=O)C(C)(C)CCCOc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1
O.C(C1=CC=CC=C1)(=O)C1=CC2=C(N=CS2=O)C=C1.C(=O)([O-])[O-].[K+].[K+].ClCCOC1=CC=C(OCCCC(C(=O)OCC)(C)C)C=C1>>C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OCCCC(C(=O)OCC)(C)C)C=C2)C=C1
Cl[CH2:19][CH2:18][O:17][c:16]1[cH:15][cH:14][c:13]([O:12][CH2:11][CH2:10][CH2:9][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH3:8])[cH:39][cH:38]1.[N:20]1=[CH:21][S:23](=[O:22])[c:24]2[cH:25][c:26]([C:27](=[O:28])[c:29]3[cH:30][cH:31][cH:32][cH:33][cH:34]3)[cH:35][cH:36][c:37]21>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[...
CCOC(=O)C(C)(C)CCCOc1ccc(OCCCl)cc1.O=C(c1ccccc1)c1ccc2c(c1)S(=O)C=N2
CCOC(=O)C(C)(C)CCCOc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1
null
null
CN(C)C=O
Heteroatom Alkylation and Arylation
OtherReaction
42c83f048334b1ed148ed7afdbd743f45dba21a36b3061112c38545e7e60436d
3dcb031a7507da808ae5e1b8f13ca2c4f0152648164857a941ec9d83076e2a56
O=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
Cl-[CH2;D2;+0:1]-[C:2]-[#8:3].[O;H0;D1;+0:4]=[S;H0;D3;+0:5]1-[CH;D2;+0:6]=[N;H0;D2;+0:7]-[c:8](:[c:9]):[c:10]-1:[c:11]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:7]1:[c:8](:[c:9]):[c:10](:[c:11]):[s;H0;D2;+0:5]:[c;H0;D3;+0:6]:1=[O;H0;D1;+0:4]
null
[]
120
CELSIUS
null
null
To a solution, heated at 80° C. for 2 hours, of 6-benzoyl-benzothiazolinone (1 g) in the presence of K2CO3 (1.08 g) in 10 ml of DMF there is added ethyl 5-[4-(2-chloroethoxy)phenoxy]-2,2-dimethylpentanoate (1.41 g). The reaction mixture is heated at 120° C. for 5 days and is then hydrolysed using 100 ml of water. The s...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Sulfoxide
null
c1ccc2scnc2c1
c1ccc2scnc2c1
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HCl
CN(C)C=O
120
null
CCOC(=O)C(C)(C)CCCOc1ccc(OCCCl)cc1.O=C(c1ccccc1)c1ccc2c(c1)S(=O)C=N2>CN(C)C=O>CCOC(=O)C(C)(C)CCCOc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-52ded71733214fc18f24b59c99b12ca7
CCOC(=O)C(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CCOC(=O)C(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)C)C=C2)C=C1.CON>>CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)C)C=C2)C=C1)C1=CC=CC=C1
O=[C:23]([c:22]1[cH:21][c:20]2[s:19][c:17](=[O:18])[n:16]([CH2:15][CH2:14][O:13][c:12]3[cH:11][cH:10][c:9]([O:8][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH3:7])[cH:37][cH:36]3)[c:35]2[cH:34][cH:33]1)[c:27]1[cH:28][cH:29][cH:30][cH:31][cH:32]1.[NH2:24][O:25][CH3:26]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH3:7])[O:8][...
CCOC(=O)C(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON
CCOC(=O)C(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step A, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-methylhydroxylamine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
null
null
null
CCOC(=O)C(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CCOC(=O)C(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8abf8f58a68546f390b521c3721265a9
CCOC(=O)C(CC)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CCOC(=O)C(CC)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)CC)C=C2)C=C1.CON>>CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)CC)C=C2)C=C1)C1=CC=CC=C1
O=[C:24]([c:23]1[cH:22][c:21]2[s:20][c:18](=[O:19])[n:17]([CH2:16][CH2:15][O:14][c:13]3[cH:12][cH:11][c:10]([O:9][CH:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])[CH2:7][CH3:8])[cH:38][cH:37]3)[c:36]2[cH:35][cH:34]1)[c:28]1[cH:29][cH:30][cH:31][cH:32][cH:33]1.[NH2:25][O:26][CH3:27]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH:6]([CH2:7...
CCOC(=O)C(CC)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON
CCOC(=O)C(CC)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step A, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-methylhydroxylamine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
null
null
null
CCOC(=O)C(CC)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1.CON>>CCOC(=O)C(CC)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4ccccc4)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-26fc786b3d5346d4a077959ef5fcb4b9
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(C)=O)ccc32)cc1.CON>>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(C)=NOC)ccc32)cc1
C(C)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1.CON>>CON=C(C)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(OC(C(=O)OCC)(C)C)C=C2)C=C1
O=[C:24]([c:23]1[cH:22][c:21]2[s:20][c:18](=[O:19])[n:17]([CH2:16][CH2:15][O:14][c:13]3[cH:12][cH:11][c:10]([O:9][C:6]([C:4]([O:3][CH2:2][CH3:1])=[O:5])([CH3:7])[CH3:8])[cH:33][cH:32]3)[c:31]2[cH:30][cH:29]1)[CH3:25].[NH2:26][O:27][CH3:28]>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[C:6]([CH3:7])([CH3:8])[O:9][c:10]1[cH:11][cH:1...
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(C)=O)ccc32)cc1.CON
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(C)=NOC)ccc32)cc1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
O=c1sc2ccccc2n1CCOc1ccccc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[c:3](:[c:4]):[c:5]:[c:6]:[#16;a:7].[C;D1;H3:8]-[#8:9]-[NH2;D1;+0:10]>>[#16;a:7]:[c:6]:[c:5]:[c:3](-[C;H0;D3;+0:1](-[C;D1;H3:2])=[N;H0;D2;+0:10]-[#8:9]-[C;D1;H3:8]):[c:4]
null
[]
null
null
null
null
Starting from the compound obtained in Step A, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-methylhydroxylamine. The two (Z) and (E) compounds are not separated. Conditions: See reaction.notes.procedure_details. Workup: The two (Z) and (E) compounds are not separated
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1
HO-
null
null
null
CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(C)=O)ccc32)cc1.CON>>CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(C)=NOC)ccc32)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8806e84ee0fb48c0ae41a84d9c3dcbae
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1)C(=O)OC.CON>>CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4cccc(Cl)c4)ccc32)cc1)C(=O)OC
ClC=1C=C(C(=O)C2=CC3=C(N(C(S3)=O)CCOC3=CC=C(C=C3)CC(C(=O)OC)OCC)C=C2)C=CC1.CON>>ClC=1C=C(C=CC1)C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)OC)OCC)C=C1)=NOC
O=[C:20]([c:19]1[cH:18][c:17]2[s:16][c:14](=[O:15])[n:13]([CH2:12][CH2:11][O:10][c:9]3[cH:8][cH:7][c:6]([CH2:5][CH:4]([O:3][CH2:2][CH3:1])[C:36](=[O:37])[O:38][CH3:39])[cH:35][cH:34]3)[c:33]2[cH:32][cH:31]1)[c:24]1[cH:25][cH:26][cH:27][c:28]([Cl:29])[cH:30]1.[NH2:21][O:22][CH3:23]>>[CH3:1][CH2:2][O:3][CH:4]([CH2:5][c:6...
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1)C(=O)OC.CON
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4cccc(Cl)c4)ccc32)cc1)C(=O)OC
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C;D1;H3:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step A, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-methylhydroxylamine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
null
null
null
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1)C(=O)OC.CON>>CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4cccc(Cl)c4)ccc32)cc1)C(=O)OC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e7d06a53b0af464291e716e56b46128e
CC(C)(C)ON.CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)C(=O)OC>>CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOC(C)(C)C)c4ccccc4)ccc32)cc1)C(=O)OC
C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)OC)OCC)C=C1.C(C)(C)(C)ON>>C(C)(C)(C)ON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)OC)OCC)C=C1)C1=CC=CC=C1
[NH2:21][O:22][C:23]([CH3:24])([CH3:25])[CH3:26].O=[C:20]([c:19]1[cH:18][c:17]2[s:16][c:14](=[O:15])[n:13]([CH2:12][CH2:11][O:10][c:9]3[cH:8][cH:7][c:6]([CH2:5][CH:4]([O:3][CH2:2][CH3:1])[C:38](=[O:39])[O:40][CH3:41])[cH:37][cH:36]3)[c:35]2[cH:34][cH:33]1)[c:27]1[cH:28][cH:29][cH:30][cH:31][cH:32]1>>[CH3:1][CH2:2][O:3]...
CC(C)(C)ON.CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)C(=O)OC
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOC(C)(C)C)c4ccccc4)ccc32)cc1)C(=O)OC
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C;D1;H3:10]-[C:11](-[C;D1;H3:12])(-[C;D1;H3:13])-[#8:14]-[NH2;D1;+0:15]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:15]-[#8:14]-[C:11](-[C;D1;H3:10])(-[C;D1;H3:12])-[C;D1;H3:13])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step C of Example 1, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-(tert-butyl)hydroxylamine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
HO-
null
null
null
CC(C)(C)ON.CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)C(=O)OC>>CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOC(C)(C)C)c4ccccc4)ccc32)cc1)C(=O)OC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e2c294d2b5db404aa07425636a9c1607
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)C(=O)OC.NOCc1ccccc1>>CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOCc4ccccc4)c4ccccc4)ccc32)cc1)C(=O)OC
C(C1=CC=CC=C1)(=O)C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)OC)OCC)C=C1.C(C1=CC=CC=C1)ON>>C(C1=CC=CC=C1)ON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)OC)OCC)C=C1)C1=CC=CC=C1
O=[C:20]([c:19]1[cH:18][c:17]2[s:16][c:14](=[O:15])[n:13]([CH2:12][CH2:11][O:10][c:9]3[cH:8][cH:7][c:6]([CH2:5][CH:4]([O:3][CH2:2][CH3:1])[C:41](=[O:42])[O:43][CH3:44])[cH:40][cH:39]3)[c:38]2[cH:37][cH:36]1)[c:30]1[cH:31][cH:32][cH:33][cH:34][cH:35]1.[NH2:21][O:22][CH2:23][c:24]1[cH:25][cH:26][cH:27][cH:28][cH:29]1>>[C...
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)C(=O)OC.NOCc1ccccc1
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOCc4ccccc4)c4ccccc4)ccc32)cc1)C(=O)OC
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
3d7a74a3d1c5abb5292963d4a3067f1fb8a89aead752dc9bb1d63522c4c0bd5c
6b0edeaa66853687109d0d530554f76edf36b01a8ec084e7ae9c709f0949a6b9
O=c1sc2cc(C(=NOCc3ccccc3)c3ccccc3)ccc2n1CCOc1ccccc1
O=[C;H0;D3;+0:1](-[c:2](:[c:3]):[c:4]:[c:5]:[#16;a:6])-[c:7](:[c:8]):[c:9].[C:10]-[#8:11]-[NH2;D1;+0:12]>>[#16;a:6]:[c:5]:[c:4]:[c:2](-[C;H0;D3;+0:1](=[N;H0;D2;+0:12]-[#8:11]-[C:10])-[c:7](:[c:8]):[c:9]):[c:3]
null
[]
null
null
null
null
Starting from the compound obtained in Step C of Example 1, the procedure is as in Step B of Example 2, replacing the hydroxylamine by O-benzylhydroxylamine. Conditions: See reaction.notes.procedure_details.
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1.c1ccccc1
HO-
null
null
null
CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=O)c4ccccc4)ccc32)cc1)C(=O)OC.NOCc1ccccc1>>CCOC(Cc1ccc(OCCn2c(=O)sc3cc(C(=NOCc4ccccc4)c4ccccc4)ccc32)cc1)C(=O)OC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-19b7ee442f184e3aac6214417427587e
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(OCC(F)(F)F)C(=O)O)cc1>>CO/N=C(/c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(OCC(F)(F)F)C(=O)O)cc1
CON=C(C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)O)OCC(F)(F)F)C=C1)C1=CC=CC=C1>>CO\N=C(/C1=CC2=C(N(C(S2)=O)CCOC2=CC=C(C=C2)CC(C(=O)O)OCC(F)(F)F)C=C1)\C1=CC=CC=C1
[CH3:1][O:2][N:3]=[C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)[c:11]1[cH:12][cH:13][c:14]2[c:15]([cH:16]1)[s:17][c:18](=[O:19])[n:20]2[CH2:21][CH2:22][O:23][c:24]1[cH:25][cH:26][c:27]([CH2:28][CH:29]([O:30][CH2:31][C:32]([F:33])([F:34])[F:35])[C:36](=[O:37])[OH:38])[cH:39][cH:40]1>>[CH3:1][O:2]/[N:3]=[C:4](/[c:5]1[cH:...
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(OCC(F)(F)F)C(=O)O)cc1
CO/N=C(/c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(OCC(F)(F)F)C(=O)O)cc1
null
null
C(C)OCC
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
N=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccccc1
null
null
[]
null
null
null
null
The compound obtained in Example 62 is taken up in the diethyl ether. The filtrate is recovered and evaporated to yield the title compound. Conditions: See reaction.notes.procedure_details. Workup: The filtrate is recovered; evaporated
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1ccc2scnc2c1.c1ccccc1
null
C(C)OCC
null
null
CON=C(c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(OCC(F)(F)F)C(=O)O)cc1>C(C)OCC>CO/N=C(/c1ccccc1)c1ccc2c(c1)sc(=O)n2CCOc1ccc(CC(OCC(F)(F)F)C(=O)O)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c4fb685667cc4027a9ae52d41dc084f1
CO.Nc1ccc(Cl)c(C(=O)O)c1>>COC(=O)c1cc(N)ccc1Cl
NC=1C=CC(=C(C(=O)O)C1)Cl.S(O)(O)(=O)=O.CO>>COC(C1=C(C=CC(=C1)N)Cl)=O
[CH3:1][OH:2].O[C:3](=[O:4])[c:5]1[cH:6][c:7]([NH2:8])[cH:9][cH:10][c:11]1[Cl:12]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([NH2:8])[cH:9][cH:10][c:11]1[Cl:12]
CO.Nc1ccc(Cl)c(C(=O)O)c1
COC(=O)c1cc(N)ccc1Cl
null
null
null
Protection
Esterification of Carboxylic Acids
9cecdbd189c6f9c3648521d17154d013842a5498de4e76e65efb1d842973340b
af0b8064f2e82ebe66c4c29d2391785ac1b993104265ccdc4d67ca79e36fa3c8
c1ccccc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C;D1;H3:6]-[OH;D1;+0:7]>>[C;D1;H3:6]-[O;H0;D2;+0:7]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
null
[]
null
null
null
null
To a slurry of 5-amino-2-chloro-benzoic acid (20.0 g, 0.12 mol) in methanol (150 mL) was added concentrated sulfuric acid (25 mL). The resulting reaction was heated at reflux for 4 hours, cooled, and concentrated in vacuo. The residual was taken up in water and neutralized with Na2CO3. The aqueous was extracted with CH...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Methanol
Ester
null
null
c1ccccc1
HO-
null
null
null
CO.Nc1ccc(Cl)c(C(=O)O)c1>>COC(=O)c1cc(N)ccc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6da8632a0fd04031988c99538c46b5f4
COC(=O)c1cc(N)ccc1Cl>>COC(=O)c1cc(NN)ccc1Cl.Cl
COC(C1=C(C=CC(=C1)N)Cl)=O.O.O.Cl[Sn]Cl.C(C)(=O)O.N(=O)[O-].[Na+]>>Cl.COC(C1=C(C=CC(=C1)NN)Cl)=O
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([NH2:8])[cH:10][cH:11][c:12]1[Cl:13]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([NH:8][NH2:9])[cH:10][cH:11][c:12]1[Cl:13].[ClH:14]
COC(=O)c1cc(N)ccc1Cl
COC(=O)c1cc(NN)ccc1Cl.Cl
null
null
Cl.O
Miscellaneous
OtherReaction
c4079cd46dafde13b56adeac363106820ab4184dee8b1ca632594de2bba804bd
5c8e4e590249a630a16b10bd7a77b27600fffbea367a0b585a920dd877e5471b
c1ccccc1
[NH2;D1;+0:1]-[c:2](:[c:3]):[c:4]>>[N;D1;H2:5]-[NH;D2;+0:1]-[c:2](:[c:3]):[c:4]
183.3
[{"value": 183.3, "product": "Cl.COC(C1=C(C=CC(=C1)NN)Cl)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
15
MINUTE
To 5-amino-2-chloro-benzoic acid methyl ester (14.0 g, 75.0 mmol) in water (100 mL) was added concentrated HCl (100 mL), followed by glacial acetic acid (100 mL). The solution was stirred at ambient temperature for 15 minutes. The reaction was then cooled to 0° C., and a solution of sodium nitrite (5.69, 82.5 mmol) in ...
10.6084/m9.figshare.5104873.v1
null
Primary amine
Hydrazine
null
null
c1ccccc1
Other
Cl.O
null
0.25
COC(=O)c1cc(N)ccc1Cl>Cl.O>COC(=O)c1cc(NN)ccc1Cl.Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a6440d65e9064d14ad3fc361a82b8d96
COC(=O)c1cc(NN)ccc1Cl.O=CC(=O)O>>COC(=O)c1cc(NN=CC(=O)O)ccc1Cl
Cl.COC(C1=C(C=CC(=C1)NN)Cl)=O.O=CC(=O)O>>COC(C1=C(C=CC(=C1)NN=CC(=O)O)Cl)=O
[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([NH:8][NH2:9])[cH:14][cH:15][c:16]1[Cl:17].O=[CH:10][C:11](=[O:12])[OH:13]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([NH:8][N:9]=[CH:10][C:11](=[O:12])[OH:13])[cH:14][cH:15][c:16]1[Cl:17]
COC(=O)c1cc(NN)ccc1Cl.O=CC(=O)O
COC(=O)c1cc(NN=CC(=O)O)ccc1Cl
null
null
Cl
Heteroatom Alkylation and Arylation
OtherReaction
c78be09cf200f3a07b02946ce0bbc22b647e9aaae7494d0480373904a4f330a9
c3cbc07b90655a7aa9777b584274a03a2ec0cff34c5b5edc214a16916fe29f1c
c1ccccc1
O=[CH;D2;+0:1]-[C:2](=[O;D1;H0:3])-[O;D1;H1:4].[NH2;D1;+0:5]-[#7:6]-[c:7]>>[O;D1;H0:3]=[C:2](-[O;D1;H1:4])-[CH;D2;+0:1]=[N;H0;D2;+0:5]-[#7:6]-[c:7]
null
[]
null
null
1.5
HOUR
2-Chloro-5-hydrazino-benzoic acid methyl ester hydrochloride salt (2.0 g, 8.5 mmol) and oxoacetic acid (1.0 g, 10 mmol) were taken up in 10% HCl and stirred at ambient temperature for 1.5 hours. The resulting orange precipitate was collected by filtration. The filter cake was taken up in EtOAc, washed with brine, and d...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Aldehyde
Hydrazone
null
null
c1ccccc1
HO-
Cl
null
1.5
COC(=O)c1cc(NN)ccc1Cl.O=CC(=O)O>Cl>COC(=O)c1cc(NN=CC(=O)O)ccc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-65a98d94232b4a8dbc1370dbf320c0ca
COC(=O)c1cc(-n2nc[nH]c2=O)ccc1Cl.NCC1(O)CCCCCC1>>O=C(NCC1(O)CCCCCC1)c1cc(-n2nc[nH]c2=O)ccc1Cl
COC(C1=C(C=CC(=C1)N1N=CNC1=O)Cl)=O.Cl.NCC1(CCCCCC1)O.C1=CN(C=N1)C(=O)N2C=CN=C2.C=1C=CC2=C(C1)N=NN2O>>ClC1=C(C(=O)NCC2(CCCCCC2)O)C=C(C=C1)N1N=CNC1=O
CO[C:2](=[O:1])[c:13]1[cH:14][c:15](-[n:16]2[n:17][cH:18][nH:19][c:20]2=[O:21])[cH:22][cH:23][c:24]1[Cl:25].[NH2:3][CH2:4][C:5]1([OH:6])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1>>[O:1]=[C:2]([NH:3][CH2:4][C:5]1([OH:6])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]1)[c:13]1[cH:14][c:15](-[n:16]2[n:17][cH:18][nH:19][...
COC(=O)c1cc(-n2nc[nH]c2=O)ccc1Cl.NCC1(O)CCCCCC1
O=C(NCC1(O)CCCCCC1)c1cc(-n2nc[nH]c2=O)ccc1Cl
null
CN(C)C=1C=CN=CC1
CN(C)C=O
Acylation
Aminolysis of esters
04c54ce22aa9bc0cea0de3d900446bcab51cf02bebeb606fa788a47dcd0e37ff
4335147c9ad02004b7c12428d7eac0b2e7e0e2017adc471d01c387239de8017d
O=C(NCC1CCCCCC1)c1cccc(-n2nc[nH]c2=O)c1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5].[C:6]-[C:7]-[NH2;D1;+0:8]>>[C:6]-[C:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[c:5]
null
[]
null
null
3
HOUR
To 2-chloro-5-(5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl)-benzoic acid methyl ester (48.0 mg, 0.2 mmol) in DMF (3 mL) was added 1-aminomethyl-cycloheptanol HCl (54.0 mg, 0.3 mmol), polymer-supported CDI (660 mg, 0.6 mmol), polymer-supported DMAP (280 mg, 0.20 mmol), and HOBt (40.0 mg, 0.3 mmol). The resulting reaction was ...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Secondary amide
null
null
C1CCCCCC1.c1ccccc1.c1nc[nH]n1
HO-
CN(C)C=1C=CN=CC1.CN(C)C=O
null
3
COC(=O)c1cc(-n2nc[nH]c2=O)ccc1Cl.NCC1(O)CCCCCC1>CN(C)C=1C=CN=CC1.CN(C)C=O>O=C(NCC1(O)CCCCCC1)c1cc(-n2nc[nH]c2=O)ccc1Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d7b0d0dd863f4f7a88433015679f4e3f
COCCBr.O=C(NCC1(O)CCCCCC1)c1cc(-n2nc[nH]c2=O)ccc1Cl>>COCCn1cnn(-c2ccc(Cl)c(C(=O)NCC3(O)CCCCCC3)c2)c1=O
ClC1=C(C(=O)NCC2(CCCCCC2)O)C=C(C=C1)N1N=CNC1=O.C(=O)([O-])[O-].[Cs+].[Cs+].COCCBr>>ClC1=C(C(=O)NCC2(CCCCCC2)O)C=C(C=C1)N1N=CN(C1=O)CCOC
Br[CH2:4][CH2:3][O:2][CH3:1].[nH:5]1[cH:6][n:7][n:8](-[c:9]2[cH:10][cH:11][c:12]([Cl:13])[c:14]([C:15](=[O:16])[NH:17][CH2:18][C:19]3([OH:20])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]3)[cH:27]2)[c:28]1=[O:29]>>[CH3:1][O:2][CH2:3][CH2:4][n:5]1[cH:6][n:7][n:8](-[c:9]2[cH:10][cH:11][c:12]([Cl:13])[c:14]([C:15](=[O:...
COCCBr.O=C(NCC1(O)CCCCCC1)c1cc(-n2nc[nH]c2=O)ccc1Cl
COCCn1cnn(-c2ccc(Cl)c(C(=O)NCC3(O)CCCCCC3)c2)c1=O
null
null
O.CS(=O)C
Heteroatom Alkylation and Arylation
N-alkylation of secondary amines with alkyl halides
8bef00eaa42d3c717b13b9e6e5eb0aaa548aa02b0e5b8a7323f70bc5d1c7c865
2e1e5fd9557b69cb528f6b2ffd179c67ef24ecb1a2c3994e1cdf0efe7ae19e9c
O=C(NCC1CCCCCC1)c1cccc(-n2nc[nH]c2=O)c1
Br-[CH2;D2;+0:1]-[C:2]-[#8:3].[O;D1;H0:4]=[c:5]1:[nH;D2;+0:6]:[c:7]:[#7;a:8]:[#7;a:9]:1-[c:10]>>[#8:3]-[C:2]-[CH2;D2;+0:1]-[n;H0;D3;+0:6]1:[c:7]:[#7;a:8]:[#7;a:9](-[c:10]):[c:5]:1=[O;D1;H0:4]
34.9
[{"value": 34.9, "product": "ClC1=C(C(=O)NCC2(CCCCCC2)O)C=C(C=C1)N1N=CN(C1=O)CCOC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
48
HOUR
A slurry of 2-Chloro-N-(1-hydroxy-cycloheptylmethyl)-5-(5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl)-benzamide (44.4 mg, 0.122 mmol) and Cs2CO3 (66.0 mg, 0.202 mmol) were stirred in DMSO (0.813 mL) at ambient temperature for 20 minutes. 2-Bromoethyl methyl ether (17.0 mg, 0.122 mmol) was added and the reaction stirred at amb...
10.6084/m9.figshare.5104873.v1
null
Primary halide
null
c1nnc[nH]1
c1nnc[nH]1
c1nnc[nH]1.c1ccccc1.C1CCCCCC1
HBr
O.CS(=O)C
null
48
COCCBr.O=C(NCC1(O)CCCCCC1)c1cc(-n2nc[nH]c2=O)ccc1Cl>O.CS(=O)C>COCCn1cnn(-c2ccc(Cl)c(C(=O)NCC3(O)CCCCCC3)c2)c1=O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6261267f2f8e4379be277cdae9ecfd82
N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1>>N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1
C(C1=CC=CC=C1)N1C[C@@H](CC1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C#N.Cl>>Cl.C(C1=CC=CC=C1)N1C[C@@H](CC1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C#N
[N:2]#[C:3][C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[C@@H:17]1[CH2:18][CH2:19][N:20]([CH2:21][c:22]2[cH:23][cH:24][cH:25][cH:26][cH:27]2)[CH2:28]1>>[N:2]#[C:3][C:4]([c:5]1[cH:6][cH:7][cH:8][cH:9][cH:10]1)([c:11]1[cH:12][cH:13][cH:14][cH:15][cH:16]1)[C@@H:17]1[CH2:18][CH2...
N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1
N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1
null
null
null
Miscellaneous
OtherReaction
40ba59785861b8226ce5af6bdcbb9a37f0ff50a8c7ec7d4fc4c524cf906cc65c
56ebed4a8b3cebec83c37a71d68f0c87d1e404ab05a9ce792691e4e18a2379dd
c1ccc(CN2CC[C@@H](C(c3ccccc3)c3ccccc3)C2)cc1
null
null
[]
null
null
null
null
(S)-1-Benzyl-3-(1-cyano-1,1-diphenylmethyl)pyrrolidine was dissolved in IPAc (approximately 1 g/10 mL) and the solution was mixed with an equal volume of 1N aqueous HCl. The resulting layers were separated and the aqueous layer was extracted with an equal volume of IPAc. The organic layers were combined, dried over sod...
10.6084/m9.figshare.5104873.v1
null
null
null
null
null
c1ccccc1.c1ccccc1.C1CC[NH]C1.c1ccccc1
null
null
null
null
N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1>>N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b8801616301c4e96a73b970a3e9c4467
N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1>>N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCNC1
Cl.C(C1=CC=CC=C1)N1C[C@@H](CC1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C#N.C(=O)[O-].[NH4+].O>>C(#N)C(C1=CC=CC=C1)(C1=CC=CC=C1)[C@H]1CNCC1
c1ccc(C[N:19]2[CH2:18][CH2:17][C@@H:16]([C:3]([C:2]#[N:1])([c:4]3[cH:5][cH:6][cH:7][cH:8][cH:9]3)[c:10]3[cH:11][cH:12][cH:13][cH:14][cH:15]3)[CH2:20]2)cc1>>[N:1]#[C:2][C:3]([c:4]1[cH:5][cH:6][cH:7][cH:8][cH:9]1)([c:10]1[cH:11][cH:12][cH:13][cH:14][cH:15]1)[C@@H:16]1[CH2:17][CH2:18][NH:19][CH2:20]1
N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1
N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCNC1
null
[Pd]
CO
Deprotection
Hydrogenolysis of tertiary amines
846a35f8c83fa58d2c714915319a8bc96745602a4dd9ac20dbad14bc1e16a470
1c99dd446c0bf4ae872cd8df8de34955be195747c234e9f3c49f46d1de614f66
c1ccc(C(c2ccccc2)[C@@H]2CCNC2)cc1
C(-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[C:4]-[C:5]-1)-c1:c:c:c:c:c:1>>[C:4]1-[C:3]-[C:2]-[NH;D2;+0:1]-[C:5]-1
99.7
[{"value": 99.7, "product": "C(#N)C(C1=CC=CC=C1)(C1=CC=CC=C1)[C@H]1CNCC1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 99.7, "product": "C(#N)C(C1=CC=CC=C1)(C1=CC=CC=C1)[C@H]1CNCC1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
50
CELSIUS
3
HOUR
To a stirred solution of (S)-1-benzyl-3-(1-cyano-1,1-diphenylmethyl)-pyrrolidine hydrochloride (8.55 g, 21.98 mmol) in MeOH (44 mL) was added palladium on carbon (1.71 g) and ammonium formate (6.93 g, 109.9 mmol). The reaction mixture was heated to 50° C. with stirring for 3 hours. The reaction was cooled to ambient te...
10.6084/m9.figshare.5104873.v1
null
Tertiary amine
Secondary amine
c1ccccc1.C1CC[NH]C1
C1CCNC1
c1ccccc1.c1ccccc1.C1CCNC1
Other
[Pd].CO
50
3
N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCN(Cc2ccccc2)C1>[Pd].CO>N#CC(c1ccccc1)(c1ccccc1)[C@@H]1CCNC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-598b57d4432c433ab63bb311f3240ad0
CN(CC(=O)NCCCCCN1CC[C@@H](C(C(N)=O)(c2ccccc2)c2ccccc2)C1)C(=O)OC(C)(C)C>>CNCC(=O)NCCCCCN1CC[C@@H](C(C(N)=O)(c2ccccc2)c2ccccc2)C1
C(C)(C)(C)OC(N(C)CC(NCCCCCN1C[C@@H](CC1)C(C1=CC=CC=C1)(C1=CC=CC=C1)C(N)=O)=O)=O.Cl.C(=O)(C(F)(F)F)O>>CNCC(=O)NCCCCCN1C[C@@H](CC1)C(C(=O)N)(C1=CC=CC=C1)C1=CC=CC=C1
CC(C)(C)OC(=O)[N:2]([CH3:1])[CH2:3][C:4](=[O:5])[NH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][N:12]1[CH2:13][CH2:14][C@@H:15]([C:16]([C:17]([NH2:18])=[O:19])([c:20]2[cH:21][cH:22][cH:23][cH:24][cH:25]2)[c:26]2[cH:27][cH:28][cH:29][cH:30][cH:31]2)[CH2:32]1>>[CH3:1][NH:2][CH2:3][C:4](=[O:5])[NH:6][CH2:7][CH2:8][CH2:9][CH2:...
CN(CC(=O)NCCCCCN1CC[C@@H](C(C(N)=O)(c2ccccc2)c2ccccc2)C1)C(=O)OC(C)(C)C
CNCC(=O)NCCCCCN1CC[C@@H](C(C(N)=O)(c2ccccc2)c2ccccc2)C1
null
null
O1CCOCC1.C(Cl)Cl
Reduction
Boc amine deprotection
bbda4640db5f48af4538caded12fdadd56eacd6d4e5f7aefe46282d665df167e
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc(C(c2ccccc2)[C@@H]2CCNC2)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C;D1;H3:2])-[C:3]-[C:4](=[O;D1;H0:5])-[#7:6]-[C:7]>>[C:7]-[#7:6]-[C:4](=[O;D1;H0:5])-[C:3]-[NH;D2;+0:1]-[C;D1;H3:2]
91.7
[{"value": 91.7, "product": "CNCC(=O)NCCCCCN1C[C@@H](CC1)C(C(=O)N)(C1=CC=CC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
To a stirred solution of ({5-[(S)-3-(carbamoyldiphenylmethyl)pyrrolidin-1-yl]pentylcarbamoyl}methyl)methylcarbamic acid tert-butyl ester (23.47 g, 43.7 mmol) in DCM (60 mL) was added 4 N HCl in dioxane (100 mL). The reaction mixture was stirred at room temperature for 2 hours and then concentrated to dryness. The resid...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
null
null
C1CC[NH]C1.c1ccccc1.c1ccccc1
HO-
O1CCOCC1.C(Cl)Cl
null
2
CN(CC(=O)NCCCCCN1CC[C@@H](C(C(N)=O)(c2ccccc2)c2ccccc2)C1)C(=O)OC(C)(C)C>O1CCOCC1.C(Cl)Cl>CNCC(=O)NCCCCCN1CC[C@@H](C(C(N)=O)(c2ccccc2)c2ccccc2)C1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c5390d5a8a25467485038a2668f38edf
COc1ccc(OC)c2ccccc12>>COc1cc(C=O)c(OC)c2ccccc12
O.COC1=CC=C(C2=CC=CC=C12)OC.COC(Cl)Cl>>COC1=C(C=C(C2=CC=CC=C12)OC)C=O
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:8]([O:9][CH3:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]12>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH:6]=[O:7])[c:8]([O:9][CH3:10])[c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]12
COc1ccc(OC)c2ccccc12
COc1cc(C=O)c(OC)c2ccccc12
null
null
ClCCl
Miscellaneous
OtherReaction
67ced7cb99084202a37bff5e70c1f0d5ea491cac26940b361bc4195cc20b94d1
3cccf922e74135722ee21a46ad7578302a8603e1f71d6f2113cd42de4ba0cf73
c1ccc2ccccc2c1
[#8:1]-[c:2](:[c:3]):[cH;D2;+0:4]:[c:5]:[c:6]>>[#8:1]-[c:2](:[c:3]):[c;H0;D3;+0:4](-[C:7]=[O;D1;H0:8]):[c:5]:[c:6]
null
[]
null
null
30
MINUTE
To a solution of 1,4-dimethoxy-naphthalene (5 g, 26.6 mmol) in dichloromethane (100 mL) at 0° C. was added dichloromethyl methyl ether (3.66 g, 31.9 mmol) and stannic chloride (13.8 g, 53.1 mmol). The reaction mixture was stirred for 30 min at this temperature, allowed to warm to room temperature and stirred for an add...
10.6084/m9.figshare.5104873.v1
null
null
Aldehyde
c1ccc2ccccc2c1
c1ccc2ccccc2c1
c1ccc2ccccc2c1
Other
ClCCl
null
0.5
COc1ccc(OC)c2ccccc12>ClCCl>COc1cc(C=O)c(OC)c2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-376d69b127ad44a48115925c1173cab5
CC[N+](=O)[O-].COc1cc(C=O)c(OC)c2ccccc12>>COc1cc(C=C(C)[N+](=O)[O-])c(OC)c2ccccc12
COC1=C(C=C(C2=CC=CC=C12)OC)C=O.C(C)(=O)[O-].[NH4+].[N+](=O)([O-])CC>>COC1=C(C=C(C2=CC=CC=C12)OC)C=C(C)[N+](=O)[O-]
[CH2:7]([CH3:8])[N+:9](=[O:10])[O-:11].O=[CH:6][c:5]1[cH:4][c:3]([O:2][CH3:1])[c:20]2[c:15]([c:12]1[O:13][CH3:14])[cH:16][cH:17][cH:18][cH:19]2>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH:6]=[C:7]([CH3:8])[N+:9](=[O:10])[O-:11])[c:12]([O:13][CH3:14])[c:15]2[cH:16][cH:17][cH:18][cH:19][c:20]12
CC[N+](=O)[O-].COc1cc(C=O)c(OC)c2ccccc12
COc1cc(C=C(C)[N+](=O)[O-])c(OC)c2ccccc12
null
null
null
C-C Coupling
OtherReaction
7ede86d40d3d69f429dde089476c8b7ffa9b74bf3050590255e6323d013c2daf
f736727903c0ad5511d468246b8e380897fd19905174c118ffa4ed4d3651f6ea
c1ccc2ccccc2c1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C;D1;H3:5]-[CH2;D2;+0:6]-[#7;+:7](-[O;-;D1;H0:8])=[O;D1;H0:9]>>[C;D1;H3:5]-[C;H0;D3;+0:6](=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[#7;+:7](-[O;-;D1;H0:8])=[O;D1;H0:9]
null
[]
60
CELSIUS
8
HOUR
To a solution of the product from Step A (0.8 g, 2.93 mmol) in nitroethane (10 mL) was added ammonium acetate (0.45 g, 5.84 mmol). The mixture was stirred at 60° C. overnight. The excess nitroethane was removed and the residue purified by flash chromatography (silica gel, ethyl acetate/hexane: 0.5/9.5) to give 0.5 g of...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Nitro group
Enamine
null
null
c1ccc2ccccc2c1
HO-
null
60
8
CC[N+](=O)[O-].COc1cc(C=O)c(OC)c2ccccc12>>COc1cc(C=C(C)[N+](=O)[O-])c(OC)c2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-a8b3689f37c24bc3bfcb44a80276c1aa
COc1cc(C=C(C)[N+](=O)[O-])c(OC)c2ccccc12>>COc1cc(CC(C)N)c(OC)c2ccccc12
Cl.[H-].[Al+3].[Li+].[H-].[H-].[H-].COC1=C(C=C(C2=CC=CC=C12)OC)C=C(C)[N+](=O)[O-]>>Cl.COC1=C(C=C(C2=CC=CC=C12)OC)CC(C)N
O=[N+:9]([O-])[C:7](=[CH:6][c:5]1[cH:4][c:3]([O:2][CH3:1])[c:18]2[c:13]([c:10]1[O:11][CH3:12])[cH:14][cH:15][cH:16][cH:17]2)[CH3:8]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH2:6][CH:7]([CH3:8])[NH2:9])[c:10]([O:11][CH3:12])[c:13]2[cH:14][cH:15][cH:16][cH:17][c:18]12
COc1cc(C=C(C)[N+](=O)[O-])c(OC)c2ccccc12
COc1cc(CC(C)N)c(OC)c2ccccc12
null
null
O1CCCC1.C(C)OCC
Reduction
OtherReaction
4337e4e8b75c4193a30be38c3139251eb50201a1e90dac1ecfc293dd3e226a46
1ad3bfd18d4cba7c52a6c2c4705cfa4e2dc99589d9555154a809489f21a7a436
c1ccc2ccccc2c1
O=[N+;H0;D3:1](-[O-])-[C;H0;D3;+0:2](-[C;D1;H3:3])=[CH;D2;+0:4]-[c:5](:[c:6]):[c:7]>>[C;D1;H3:3]-[CH;D3;+0:2](-[NH2;D1;+0:1])-[CH2;D2;+0:4]-[c:5](:[c:6]):[c:7]
null
[]
0
CELSIUS
null
null
The product from Step B (0.5 g, 1.83 mmol) was dissolved in tetrahydrofuran (50 mL). This solution was cooled to 0° C. and then a 1 M solution of lithium aluminum hydride in tetrahydrofuran (9 mL) was added. The reaction mixture was allowed to warm to room temperature and then warmed at reflux for an additional 5 h. Th...
10.6084/m9.figshare.5104873.v1
null
Enamine
Primary amine
null
null
c1ccc2ccccc2c1
Other
O1CCCC1.C(C)OCC
0
null
COc1cc(C=C(C)[N+](=O)[O-])c(OC)c2ccccc12>O1CCCC1.C(C)OCC>COc1cc(CC(C)N)c(OC)c2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e7432b3077a04dd99c20e2dcc8995da1
CCC(=O)Cl.COc1ccc(OC)c2ccccc12>>CCC(=O)c1cc(OC)c2ccccc2c1OC
O.[Cl-].[Al+3].[Cl-].[Cl-].COC1=CC=C(C2=CC=CC=C12)OC.C(CC)(=O)Cl>>COC1=C(C=C(C2=CC=CC=C12)OC)C(CC)=O
Cl[C:3]([CH2:2][CH3:1])=[O:4].[cH:5]1[cH:6][c:7]([O:8][CH3:9])[c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1[O:17][CH3:18]>>[CH3:1][CH2:2][C:3](=[O:4])[c:5]1[cH:6][c:7]([O:8][CH3:9])[c:10]2[cH:11][cH:12][cH:13][cH:14][c:15]2[c:16]1[O:17][CH3:18]
CCC(=O)Cl.COc1ccc(OC)c2ccccc12
CCC(=O)c1cc(OC)c2ccccc2c1OC
null
null
ClC(C)Cl
C-C Coupling
Friedel-Crafts acylation
12bfc1cb494a0014608d71eb38cabea029a6bf3a3526b0cc7babc0ad4f29f3e1
fe2a4a0dfbb5b71b9a065e092364c64b22b4eb1ad4d6ba2a1e8edc9d31fce3e4
c1ccc2ccccc2c1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C;D1;H3:4].[#8:5]-[c:6](:[c:7]):[cH;D2;+0:8]:[c:9]:[c:10]>>[#8:5]-[c:6](:[c:7]):[c;H0;D3;+0:8](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C;D1;H3:4]):[c:9]:[c:10]
21.5
[{"value": 21.5, "product": "COC1=C(C=C(C2=CC=CC=C12)OC)C(CC)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
To a cold solution (ice bath) of 1,4-dimethoxy-naphthalene (5 g, 26.6 mmol) in dichloroethane (100 mL) was added propionyl chloride (2.7 g, 29.3 mmol) followed by aluminum chloride (3.9 g, 29.3 mmol). After the addition was complete, the reaction mixture was allowed to warm to room temperature and stirred for 4 hr. Wat...
10.6084/m9.figshare.5104873.v1
null
Acyl halide
Ketone
c1ccc2ccccc2c1
c1ccc2ccccc2c1
c1ccc2ccccc2c1
HCl
ClC(C)Cl
null
4
CCC(=O)Cl.COc1ccc(OC)c2ccccc12>ClC(C)Cl>CCC(=O)c1cc(OC)c2ccccc2c1OC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6ac4fd3e3c5d4e6bace153926c2ac20d
CCC(=O)c1cc(OC)c2ccccc2c1OC.CCCCON=O>>COc1cc(C(=O)C(C)=NO)c(OC)c2ccccc12
Cl.COC1=C(C=C(C2=CC=CC=C12)OC)C(CC)=O.Cl.N(=O)OCCCC.N(=O)OCCCC>>COC1=C(C=C(C2=CC=CC=C12)OC)C(C(C)=NO)=O
[CH3:1][O:2][c:3]1[cH:4][c:5]([C:6](=[O:7])[CH2:8][CH3:9])[c:12]([O:13][CH3:14])[c:15]2[cH:16][cH:17][cH:18][cH:19][c:20]12.CCCCO[N:10]=[O:11]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([C:6](=[O:7])[C:8]([CH3:9])=[N:10][OH:11])[c:12]([O:13][CH3:14])[c:15]2[cH:16][cH:17][cH:18][cH:19][c:20]12
CCC(=O)c1cc(OC)c2ccccc2c1OC.CCCCON=O
COc1cc(C(=O)C(C)=NO)c(OC)c2ccccc12
null
null
C(C)OCC
Heteroatom Alkylation and Arylation
OtherReaction
977610bf44fbda1e0a23f5dd16db8b0cb303f37c36d5a67ff66ec243f6e1d15c
31357763b1be60679a29f55afc8815d0b4a90e485d09aebc6e88f16eae688399
c1ccc2ccccc2c1
C-C-C-C-O-[N;H0;D2;+0:1]=[O;H0;D1;+0:2].[C;D1;H3:3]-[CH2;D2;+0:4]-[C:5](=[O;D1;H0:6])-[c:7]>>[C;D1;H3:3]-[C;H0;D3;+0:4](=[N;H0;D2;+0:1]-[OH;D1;+0:2])-[C:5](=[O;D1;H0:6])-[c:7]
55.9
[{"value": 55.9, "product": "COC1=C(C=C(C2=CC=CC=C12)OC)C(C(C)=NO)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
4
HOUR
The product from Step A (1.28 g, 5.24 mmol) was dissolved in ethyl ether (50 mL), anhydrous hydrogen chloride gas was added through this solution at moderate rate for 5 min. Butyl nitrite (0.68 mL, 5.77 mmol) was then added dropwise. Hydrogen chloride bubbling was continued for an additional 10 min. after addition of b...
10.6084/m9.figshare.5104873.v1
null
Ketone.Nitroso
Ketone.Oxime
null
null
c1ccc2ccccc2c1
HO-
C(C)OCC
null
4
CCC(=O)c1cc(OC)c2ccccc2c1OC.CCCCON=O>C(C)OCC>COc1cc(C(=O)C(C)=NO)c(OC)c2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-0893e4388b4946148f4fb6c36f0aa994
COc1ccc(OC)c2ccccc12.C[C@@H](NC(=O)C(F)(F)F)C(=O)O>>COc1cc(C(=O)[C@@H](C)NC(=O)C(F)(F)F)c(OC)c2ccccc12
FC(C(=O)N[C@H](C)C(=O)O)(F)F.[Al+3].[Cl-].[Cl-].[Cl-].COC1=CC=C(C2=CC=CC=C12)OC>>COC1=C(C=C(C2=CC=CC=C12)OC)C([C@@H](C)NC(C(F)(F)F)=O)=O
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:17]([O:18][CH3:19])[c:20]2[cH:21][cH:22][cH:23][cH:24][c:25]12.O[C:6](=[O:7])[C@@H:8]([CH3:9])[NH:10][C:11](=[O:12])[C:13]([F:14])([F:15])[F:16]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([C:6](=[O:7])[C@@H:8]([CH3:9])[NH:10][C:11](=[O:12])[C:13]([F:14])([F:15])[F:16])[c:17]([O:18][CH3:19])[c:20]2[...
COc1ccc(OC)c2ccccc12.C[C@@H](NC(=O)C(F)(F)F)C(=O)O
COc1cc(C(=O)[C@@H](C)NC(=O)C(F)(F)F)c(OC)c2ccccc12
null
null
ClCCl.C(Cl)Cl
C-C Coupling
Friedel-Crafts acylation
6c02866b83e7a20d3fad869afb283fb288a49d5d0ad15036a6cc97e1db12cdce
a49756d2995b35bf1c4b6840928f031562470ef5bd676447fb43ce2575147daa
c1ccc2ccccc2c1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])-[#7:5]-[C:6]=[O;D1;H0:7].[#8:8]-[c:9](:[c:10]):[cH;D2;+0:11]:[c:12]:[c:13]>>[#8:8]-[c:9](:[c:10]):[c;H0;D3;+0:11](-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3](-[C;D1;H3:4])-[#7:5]-[C:6]=[O;D1;H0:7]):[c:12]:[c:13]
32.6
[{"value": 32.6, "product": "COC1=C(C=C(C2=CC=CC=C12)OC)C([C@@H](C)NC(C(F)(F)F)=O)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
To a suspension of AlCl3 (3.8 g, 28.6 mmol) in dichloromethane (100 mL) was added a solution of 1,4-dimethoxynaphthalene (4.88 g, 25.9 mmol) in dichloromethane (50 mL). To this mixture was added a solution of (R)-N-trifluoroacetylalanine (16 g, 86.5 mmol) in CH2Cl2 (50 mL); this mixture was stirred at room temperature ...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Ketone
c1ccc2ccccc2c1
c1ccc2ccccc2c1
c1ccc2ccccc2c1
HO-
ClCCl.C(Cl)Cl
null
3
COc1ccc(OC)c2ccccc12.C[C@@H](NC(=O)C(F)(F)F)C(=O)O>ClCCl.C(Cl)Cl>COc1cc(C(=O)[C@@H](C)NC(=O)C(F)(F)F)c(OC)c2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4d9520f5a9c04390ae86ba1ae95e1a5f
COS(=O)(=O)OC.O=C(O)c1ccc2ccccc2c1O>>COC(=O)c1ccc2ccccc2c1OC
S(=O)(=O)(OC)OC.OC1=C(C=CC2=CC=CC=C12)C(=O)O.C([O-])([O-])=O.[K+].[K+]>>COC1=C(C=CC2=CC=CC=C12)C(=O)OC
O=S(=O)(O[CH3:1])O[CH3:16].[OH:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[c:14]1[OH:15]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[c:14]1[O:15][CH3:16]
COS(=O)(=O)OC.O=C(O)c1ccc2ccccc2c1O
COC(=O)c1ccc2ccccc2c1OC
null
null
CC(=O)C.C(C)(=O)OCC
Heteroatom Alkylation and Arylation
OtherReaction
a73a0b4bed36565b493919c1511184d75109f6c557167d64c85b98af57b69588
edd21dfad97802e784d20c5398257e85c9ec7c075392afa5ab3339d34ce0623f
c1ccc2ccccc2c1
O=S(=O)(-O-[CH3;D1;+0:1])-O-[CH3;D1;+0:2].[O;D1;H0:3]=[C:4](-[OH;D1;+0:5])-[c:6]:[c:7](-[OH;D1;+0:8]):[c:9]>>[CH3;D1;+0:1]-[O;H0;D2;+0:8]-[c:7](:[c:9]):[c:6]-[C:4](=[O;D1;H0:3])-[O;H0;D2;+0:5]-[CH3;D1;+0:2]
90.4
[{"value": 90.4, "product": "COC1=C(C=CC2=CC=CC=C12)C(=O)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 1-hydroxy-naphthalene-2-carboxylic acid (5 g, 26.6 mmol) in acetone (100 mL) was added potassium carbonate (11 g, 79.72 mmol) followed by dimethyl sulfate (7.38 g, 58.46 mmol). The reaction mixture was refluxed overnight and then diluted with ethyl acetate (200 mL) and washed with water. The organic la...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Aromatic alcohol
Ester.Ether
null
null
c1ccc2ccccc2c1
HO-
CC(=O)C.C(C)(=O)OCC
null
null
COS(=O)(=O)OC.O=C(O)c1ccc2ccccc2c1O>CC(=O)C.C(C)(=O)OCC>COC(=O)c1ccc2ccccc2c1OC
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cd5c48fb49a04e97be2dc29a00d259d3
COC(=O)c1ccc2ccccc2c1OC>>COc1c(CO)ccc2ccccc12
C(C)(=O)OCC.[H-].[Al+3].[Li+].[H-].[H-].[H-].COC1=C(C=CC2=CC=CC=C12)C(=O)OC>>OCC1=C(C2=CC=CC=C2C=C1)OC
CO[C:5]([c:4]1[c:3]([O:2][CH3:1])[c:14]2[c:9]([cH:8][cH:7]1)[cH:10][cH:11][cH:12][cH:13]2)=[O:6]>>[CH3:1][O:2][c:3]1[c:4]([CH2:5][OH:6])[cH:7][cH:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]12
COC(=O)c1ccc2ccccc2c1OC
COc1c(CO)ccc2ccccc12
null
null
O1CCCC1
Reduction
Reduction of ester to primary alcohol
21d61543c6ec8a8cebe1b3ef55ef3dd20acbf79a4f1c12a7fb51e32be7a3248a
1fbcd628a0426673c5d10aa49a977cd2d1ae02a8cdf57bbb10d94aa03a94e937
c1ccc2ccccc2c1
C-O-[C;H0;D3;+0:1](=[O;H0;D1;+0:2])-[c:3](:[c:4]):[c:5]>>[OH;D1;+0:2]-[CH2;D2;+0:1]-[c:3](:[c:4]):[c:5]
104.6
[{"value": 104.6, "product": "OCC1=C(C2=CC=CC=C2C=C1)OC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
0
CELSIUS
30
MINUTE
The product of Step A (4.5 g, 20.83 mmol) was dissolved in anhydrous tetrahydrofuran (100 mL) and cooled to 0° C. To this solution was added a 1 M solution of lithium aluminum hydride in tetrahydrofuran (31 mL). The mixture was stirred at this temperature for 30 min, allowed to warm up to room temperature, and stirred ...
10.6084/m9.figshare.5104873.v1
null
Ester
Primary alcohol
null
null
c1ccc2ccccc2c1
Other
O1CCCC1
0
0.5
COC(=O)c1ccc2ccccc2c1OC>O1CCCC1>COc1c(CO)ccc2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c876af2d9b2c4dcc8051aa884d4c2ab1
COc1c(CO)ccc2ccccc12>>COc1c(C=O)ccc2ccccc12
OCC1=C(C2=CC=CC=C2C=C1)OC.[Cr](=O)(=O)([O-])Cl.[NH+]1=CC=CC=C1>>COC1=C(C=CC2=CC=CC=C12)C=O
[CH3:1][O:2][c:3]1[c:4]([CH2:5][OH:6])[cH:7][cH:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]12>>[CH3:1][O:2][c:3]1[c:4]([CH:5]=[O:6])[cH:7][cH:8][c:9]2[cH:10][cH:11][cH:12][cH:13][c:14]12
COc1c(CO)ccc2ccccc12
COc1c(C=O)ccc2ccccc12
null
null
ClCCl
Oxidation
Oxidation or Dehydrogenation of Alcohols to Aldehydes and Ketones
41bfa9deea81b465c88ad21fdfb64a2e1ba29490558cf430df132cb98b4a538b
0a03c6724c1862e8f86d4a463afda55b8e067dc6cb42597b472eb7cabc03eda3
c1ccc2ccccc2c1
[OH;D1;+0:1]-[CH2;D2;+0:2]-[c:3](:[c:4]):[c:5]>>[O;H0;D1;+0:1]=[CH;D2;+0:2]-[c:3](:[c:4]):[c:5]
null
[]
0
CELSIUS
1
HOUR
The product from Step B (4 g, 27.28 mmol) was dissolved in dichloromethane (100 mL) and cooled to 0° C. To this solution was added pyridinium chlorochromate (5.5 g, 25.53 mmol) and the reaction was stirred at this temperature for 1 h. The reaction mixture was washed with 1 M aqueous solution of hydrogen chloride. The o...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol
Aldehyde
null
null
c1ccc2ccccc2c1
null
ClCCl
0
1
COc1c(CO)ccc2ccccc12>ClCCl>COc1c(C=O)ccc2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cfb43091512a41c38f51122a705bcdbd
CC[N+](=O)[O-].COc1c(C=O)ccc2ccccc12>>COc1c(CC(C)N)ccc2ccccc12
[H-].[Al+3].[Li+].[H-].[H-].[H-].[N+](=O)([O-])CC.Cl.C(C)(=O)[O-].[NH4+].COC1=C(C=CC2=CC=CC=C12)C=O>>Cl.COC1=C(C=CC2=CC=CC=C12)CC(C)N
O=[N+:8]([O-])[CH2:6][CH3:7].O=[CH:5][c:4]1[c:3]([O:2][CH3:1])[c:16]2[c:11]([cH:10][cH:9]1)[cH:12][cH:13][cH:14][cH:15]2>>[CH3:1][O:2][c:3]1[c:4]([CH2:5][CH:6]([CH3:7])[NH2:8])[cH:9][cH:10][c:11]2[cH:12][cH:13][cH:14][cH:15][c:16]12
CC[N+](=O)[O-].COc1c(C=O)ccc2ccccc12
COc1c(CC(C)N)ccc2ccccc12
null
null
O1CCCC1.C(C)OCC.C(C)O
Functional Group Interconversion
OtherReaction
c4948e685a5307dbb0ab39cc775435d9f18bdf3d98a988199508e5c7eca2d454
31831dfce215791960c88ffc82ccac6c15baeee7c4c4ea60fee7e78d0106ef98
c1ccc2ccccc2c1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].O=[N+;H0;D3:5](-[O-])-[CH2;D2;+0:6]-[C;D1;H3:7]>>[C;D1;H3:7]-[CH;D3;+0:6](-[NH2;D1;+0:5])-[CH2;D2;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
70
CELSIUS
3
HOUR
The product from Step C (3.04 g, 18.3 mmol) was dissolved in ethanol (50 mL), ammonium acetate (1.55 g, 20.10 mmol) was added followed by nitroethane (2.75 g, 36.5 mmol). The reaction mixture was stirred at 70° C. for 3 h and then the solvent was removed. The residue was dissolved in ethyl acetate (100 mL) and washed w...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Nitro group
Primary amine
null
null
c1ccc2ccccc2c1
Other
O1CCCC1.C(C)OCC.C(C)O
70
3
CC[N+](=O)[O-].COc1c(C=O)ccc2ccccc12>O1CCCC1.C(C)OCC.C(C)O>COc1c(CC(C)N)ccc2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-322771b3977d4496a9db69836b0f773d
BrBr.COc1c(CC(C)N)ccc2ccccc12>>COc1c(CC(C)N)cc(Br)c2ccccc12
BrBr.Cl.COC1=C(C=CC2=CC=CC=C12)CC(C)N.FC(C(=O)OC(C(F)(F)F)=O)(F)F>>Cl.BrC1=CC(=C(C2=CC=CC=C12)OC)CC(C)N
Br[Br:11].[CH3:1][O:2][c:3]1[c:4]([CH2:5][CH:6]([CH3:7])[NH2:8])[cH:9][cH:10][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]12>>[CH3:1][O:2][c:3]1[c:4]([CH2:5][CH:6]([CH3:7])[NH2:8])[cH:9][c:10]([Br:11])[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]12
BrBr.COc1c(CC(C)N)ccc2ccccc12
COc1c(CC(C)N)cc(Br)c2ccccc12
null
null
ClCCl
Functional Group Interconversion
Bromination
3f028b3cb6667dfa94ac17841fc3d30723adc1bece1338dfafcba1f81845cc2e
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc2ccccc2c1
Br-[Br;H0;D1;+0:1].[c:2]:[c:3](:[c:4]):[cH;D2;+0:5]:[c:6]:[c:7]>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:5](:[c:6]:[c:7]):[c:3](:[c:2]):[c:4]
null
[]
0
CELSIUS
1
HOUR
To a solution of the product from Example 4 (1.2 g, 4.78 mmol) and TEA (0.97 g, 9.56 mmol) in dichloromethane (100 ml) at 0° C. was added trifluoroacetic anhydride (1.2 g, 5.74 mmol). The reaction mixture was stirred at 0° C. for 1 h and evaporated to a residue, which was filtered through silica (ethyl acetate/hexane: ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2ccccc2c1
c1ccc2ccccc2c1
c1ccc2ccccc2c1
HBr
ClCCl
0
1
BrBr.COc1c(CC(C)N)ccc2ccccc12>ClCCl>COc1c(CC(C)N)cc(Br)c2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-cde8aa8f36f64caa85bf895d0748e51a
COc1c(CC(C)N)ccc2ccccc12>>CC(N)Cc1ccc2ccccc2c1O
Cl.COC1=C(C=CC2=CC=CC=C12)CC(C)N.Br>>Cl.OC1=C(C=CC2=CC=CC=C12)CC(C)N
C[O:15][c:14]1[c:5]([CH2:4][CH:2]([CH3:1])[NH2:3])[cH:6][cH:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]21>>[CH3:1][CH:2]([NH2:3])[CH2:4][c:5]1[cH:6][cH:7][c:8]2[cH:9][cH:10][cH:11][cH:12][c:13]2[c:14]1[OH:15]
COc1c(CC(C)N)ccc2ccccc12
CC(N)Cc1ccc2ccccc2c1O
null
null
null
Deprotection
Cleavage of methoxy ethers to alcohols
c5320c7dfa4f544d4900efcae9b3262bf0d5286bcf39c86109232351f35b23d5
26a36596df80ec137b0e8087297418351c93c32819177f680675220622f215d4
c1ccc2ccccc2c1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
null
null
A solution of 2-(1-methoxy-naphthalen-2-yl)-1-methylethylamine hydrochloride (0.1 g, 0.40 mmol) and HBr 48% was refluxed for 3 h. The reaction mixture was concentrated under vacuum, the residue was washed with hexane and ether and then collected by filtration: 1H NMR (DMSO-d) δ 1.14 (d, 3H, CH3), 2.86–3.11 (m, 2H, CH2)...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccc2ccccc2c1
Other
null
null
null
COc1c(CC(C)N)ccc2ccccc12>>CC(N)Cc1ccc2ccccc2c1O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c8e7cb25be944baf86677b3c5e4b9408
COc1cc(C(=O)C(C)=NO)c(OC)c2ccccc12>>COc1cc(C(=O)C(C)N)c(OC)c2ccccc12
COC1=C(C=C(C2=CC=CC=C12)OC)C(C(C)=NO)=O.Cl.O>>Cl.NC(C(=O)C1=C(C2=CC=CC=C2C(=C1)OC)OC)C
O[N:10]=[C:8]([C:6]([c:5]1[cH:4][c:3]([O:2][CH3:1])[c:19]2[c:14]([c:11]1[O:12][CH3:13])[cH:15][cH:16][cH:17][cH:18]2)=[O:7])[CH3:9]>>[CH3:1][O:2][c:3]1[cH:4][c:5]([C:6](=[O:7])[CH:8]([CH3:9])[NH2:10])[c:11]([O:12][CH3:13])[c:14]2[cH:15][cH:16][cH:17][cH:18][c:19]12
COc1cc(C(=O)C(C)=NO)c(OC)c2ccccc12
COc1cc(C(=O)C(C)N)c(OC)c2ccccc12
null
[Pd]
C(C)O
Reduction
OtherReaction
b7ca3f61b8b30140990222f00a4d6af83c258b1760b11f7f7486b0f8e5478e46
178656017be156591ed8f29982ee3a5eb5737c28c6bf11051dfba481e2bb48a3
c1ccc2ccccc2c1
O-[N;H0;D2;+0:1]=[C;H0;D3;+0:2](-[C;D1;H3:3])-[C:4](=[O;D1;H0:5])-[c:6]>>[C;D1;H3:3]-[CH;D3;+0:2](-[NH2;D1;+0:1])-[C:4](=[O;D1;H0:5])-[c:6]
null
[]
null
null
12
HOUR
To a solution of 1-(1,4-dimethoxynaphthalen-2-yl)-propane-1,2-dione 2-oxime (1 g, 3.66 mmol, Example 2, Step B) in 1 M hydrogen chloride in ethanol (50 mL) was added Pd/C 10% (100 mg), The mixture was hydrogenated on a Parr hydrogenator apparatus under 40–50 psi pressure for 12 h. The catalyst was separated by filtrati...
10.6084/m9.figshare.5104873.v1
null
Ketone.Oxime
Ketone.Primary amine
null
null
c1ccc2ccccc2c1
Other
[Pd].C(C)O
null
12
COc1cc(C(=O)C(C)=NO)c(OC)c2ccccc12>[Pd].C(C)O>COc1cc(C(=O)C(C)N)c(OC)c2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b7b56b27075a459bb5c8651b01ad1115
BrBr.COc1cc(CC(C)N)cc2ccccc12>>COc1cc(CC(C)N)c(Br)c2ccccc12
Cl.COC1=CC(=CC2=CC=CC=C12)CC(C)N.BrBr>>Cl.BrC1=C(C=C(C2=CC=CC=C12)OC)CC(C)N
Br[Br:11].[CH3:1][O:2][c:3]1[cH:4][c:5]([CH2:6][CH:7]([CH3:8])[NH2:9])[cH:10][c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]12>>[CH3:1][O:2][c:3]1[cH:4][c:5]([CH2:6][CH:7]([CH3:8])[NH2:9])[c:10]([Br:11])[c:12]2[cH:13][cH:14][cH:15][cH:16][c:17]12
BrBr.COc1cc(CC(C)N)cc2ccccc12
COc1cc(CC(C)N)c(Br)c2ccccc12
null
null
ClCCl
Functional Group Interconversion
Bromination
3f028b3cb6667dfa94ac17841fc3d30723adc1bece1338dfafcba1f81845cc2e
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc2ccccc2c1
Br-[Br;H0;D1;+0:1].[C:2]-[c:3](:[c:4]):[cH;D2;+0:5]:[c:6](:[c:7]):[c:8]>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:5](:[c:6](:[c:7]):[c:8]):[c:3](-[C:2]):[c:4]
null
[]
null
null
null
null
To a cold heterogeneous solution (ice bath) of 2-(4-methoxy-naphthalen-2-yl) 1-methyl-ethylamine hydrochloride (0.10 g, 0.39 mmol, Example 11) in dichloromethane, was added bromine (0.07 g, 0.43 mmol) via syringe. After 1 h the volatiles were evaporated and the residue was partitioned in a mixture of ethyl acetate (20 ...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1ccc2ccccc2c1
c1ccc2ccccc2c1
c1ccc2ccccc2c1
HBr
ClCCl
null
null
BrBr.COc1cc(CC(C)N)cc2ccccc12>ClCCl>COc1cc(CC(C)N)c(Br)c2ccccc12
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e6e98be830eb44eab480e0c3b34cfda2
CCOC(=O)CBr.O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1>>CCOC(=O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
O=C1NC2=C(N1C1CCNCC1)C=CC=C2.O=C1NC2=C(N1C1CCN(CC1)CC(=O)O)C=CC=C2.BrCC(=O)OCC>>O=C1NC2=C(N1C1CCN(CC1)CC(=O)OCC)C=CC=C2
Br[CH2:6][C:4]([O:3][CH2:2][CH3:1])=[O:5].O=C(O)C[N:7]1[CH2:8][CH2:9][CH:10]([n:11]2[c:12](=[O:13])[nH:14][c:15]3[cH:16][cH:17][cH:18][cH:19][c:20]23)[CH2:21][CH2:22]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[CH2:6][N:7]1[CH2:8][CH2:9][CH:10]([n:11]2[c:12](=[O:13])[nH:14][c:15]3[cH:16][cH:17][cH:18][cH:19][c:20]23)[CH2:21][CH...
CCOC(=O)CBr.O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
CCOC(=O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
null
null
C(C)#N
Heteroatom Alkylation and Arylation
OtherReaction
80f5b5bef34a91832522456384c894e84b326f4976f8c6bb6ccd1413fa87e3b1
5e49cf00bd17391fcb272cb481c9600e6c39e7c28c33721dcc37b5cb979c7ce1
O=c1[nH]c2ccccc2n1C1CCNCC1
Br-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5].O-C(=O)-C-[N;H0;D3;+0:6](-[C:7]-[C:8])-[C:9]-[C:10]>>[C:8]-[C:7]-[N;H0;D3;+0:6](-[CH2;D2;+0:1]-[C:2](=[O;D1;H0:3])-[#8:4]-[C:5])-[C:9]-[C:10]
null
[]
null
null
null
null
Compounds of formula A in which Z=2,3-dihydro-2-oxo-1H-benzimidazol-1-yl and L=(N-methylene)piperidin-4-yl are prepared from β-aminotetralins (VII) or phenethylamines (XI) and [4-(2-keto-1-benzimidazolinyl)piperidin-1-yl]acetic acid (Schemes 6–7). For example, 4-(2-keto-1-benzimidazolinyl)piperidine is reacted with a b...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Carboxylic acid.Ester.Tertiary amine
Ester.Tertiary amine
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1.c1ccc2[nH]cnc2c1
HBr
C(C)#N
null
null
CCOC(=O)CBr.O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1>C(C)#N>CCOC(=O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-84481c84dce14da58451666086b906a5
CCOC(=O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1>>O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
O=C1NC2=C(N1C1CCN(CC1)CC(=O)OCC)C=CC=C2.[OH-].[Na+].CO>>O=C1NC2=C(N1C1CCN(CC1)CC(=O)O)C=CC=C2
CC[O:3][C:2](=[O:1])[CH2:4][N:5]1[CH2:6][CH2:7][CH:8]([n:9]2[c:10](=[O:11])[nH:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]23)[CH2:19][CH2:20]1>>[O:1]=[C:2]([OH:3])[CH2:4][N:5]1[CH2:6][CH2:7][CH:8]([n:9]2[c:10](=[O:11])[nH:12][c:13]3[cH:14][cH:15][cH:16][cH:17][c:18]23)[CH2:19][CH2:20]1
CCOC(=O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
null
null
C(C)(=O)O
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
O=c1[nH]c2ccccc2n1C1CCNCC1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
Compounds of formula A in which Z=2,3-dihydro-2-oxo-1H-benzimidazol-1-yl and L=(N-methylene)piperidin-4-yl are prepared from β-aminotetralins (VII) or phenethylamines (XI) and [4-(2-keto-1-benzimidazolinyl)piperidin-1-yl]acetic acid (Schemes 6–7). For example, 4-(2-keto-1-benzimidazolinyl)piperidine is reacted with a b...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CC[NH]CC1.c1ccc2[nH]cnc2c1
Other
C(C)(=O)O
null
null
CCOC(=O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1>C(C)(=O)O>O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b50eeddfd0eb46a38835147e8be00222
COc1ccc2c(c1)CC[C@H](NCCCCCCc1cc(N)cc(S(N)(=O)=O)c1F)[C@@H]2Cc1cccnc1.Cl>>Cl.Nc1cc(CCCCCCN[C@H]2CCc3cc(O)ccc3[C@H]2Cc2cccnc2)c(F)c(S(N)(=O)=O)c1
B(Br)(Br)Br.Cl.Cl.Cl.NC=1C=C(C(=C(C1)S(=O)(=O)N)F)CCCCCCN[C@@H]1[C@@H](C2=CC=C(C=C2CC1)OC)CC=1C=NC=CC1>>Cl.Cl.Cl.NC=1C=C(C(=C(C1)S(=O)(=O)N)F)CCCCCCN[C@@H]1[C@@H](C2=CC=C(C=C2CC1)O)CC=1C=NC=CC1
C[O:21][c:20]1[cH:19][c:18]2[c:24]([cH:23][cH:22]1)[C@@H:25]([CH2:26][c:27]1[cH:28][cH:29][cH:30][n:31][cH:32]1)[C@@H:15]([NH:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][c:7]1[cH:6][c:5]([NH2:4])[cH:40][c:35]([S:36]([NH2:37])(=[O:38])=[O:39])[c:33]1[F:34])[CH2:16][CH2:17]2.[ClH:3]>>[ClH:3].[NH2:4][c:5]1[cH:6][c:7...
COc1ccc2c(c1)CC[C@H](NCCCCCCc1cc(N)cc(S(N)(=O)=O)c1F)[C@@H]2Cc1cccnc1.Cl
Cl.Nc1cc(CCCCCCN[C@H]2CCc3cc(O)ccc3[C@H]2Cc2cccnc2)c(F)c(S(N)(=O)=O)c1
null
null
C(Cl)Cl
Miscellaneous
OtherReaction
005318874c4792a3ed14897fb19099f1f6e548b285f476e19a15213a92356c2d
0bab01685da92cdead9c84b3a9c513c0e9bd4114585991beae2460d8c47b3623
c1ccc(CCCCCCN[C@H]2CCc3ccccc3[C@H]2Cc2cccnc2)cc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
null
[]
null
null
16
HOUR
Aminotetralin sulfonamide 8 from the previous reaction (0.160 g, 0.246 mmol) was placed in a 50 mL round-bottom flask along with a stir bar. Methylene chloride (25 mL) was added and the slurry was cooled on an ice bath for several minutes. Boron tribromide in methylene chloride (1M, 1.25 mL, 1.25 mmol) was added to the...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
c1ccccc1.c1ccc2c(c1)CCCC2.c1ccncc1
Other
C(Cl)Cl
null
16
COc1ccc2c(c1)CC[C@H](NCCCCCCc1cc(N)cc(S(N)(=O)=O)c1F)[C@@H]2Cc1cccnc1.Cl>C(Cl)Cl>Cl.Nc1cc(CCCCCCN[C@H]2CCc3cc(O)ccc3[C@H]2Cc2cccnc2)c(F)c(S(N)(=O)=O)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1bcba84b1cd54f95bde7c4d8a4ae878c
COc1ccc2c(c1)CCC(N)C2Cc1cccnc1.Cl.O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1>>COc1ccc2c(c1)CC[C@H](NC(=O)CN1CCC(n3c(=O)[nH]c4ccccc43)CC1)[C@@H]2Cc1cccnc1.Cl
F[P-](F)(F)(F)(F)F.N1(N=NC2=C1C=CC=C2)OC(=[N+](C)C)N(C)C.O=C1NC2=C(N1C1CCN(CC1)CC(=O)O)C=CC=C2.C(C)(C)N(C(C)C)CC.C([O-])(O)=O.[Na+].Cl.Cl.COC=1C=C2CCC(C(C2=CC1)CC=1C=NC=CC1)N>>Cl.Cl.O=C1NC2=C(N1C1CCN(CC1)CC(=O)N[C@@H]1[C@@H](C3=CC=C(C=C3CC1)OC)CC=1C=NC=CC1)C=CC=C2
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]2[c:7]([cH:8]1)[CH2:9][CH2:10][CH:11]([NH2:12])[CH:32]2[CH2:33][c:34]1[cH:35][cH:36][cH:37][n:38][cH:39]1.[ClH:41].O[C:13](=[O:14])[CH2:15][N:16]1[CH2:17][CH2:18][CH:19]([n:20]2[c:21](=[O:22])[nH:23][c:24]3[cH:25][cH:26][cH:27][cH:28][c:29]23)[CH2:30][CH2:31]1>>[CH3:1][O:2][c:3]1[cH:4...
COc1ccc2c(c1)CCC(N)C2Cc1cccnc1.Cl.O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1
COc1ccc2c(c1)CC[C@H](NC(=O)CN1CCC(n3c(=O)[nH]c4ccccc43)CC1)[C@@H]2Cc1cccnc1.Cl
null
null
CN(C=O)C
Acylation
OtherReaction
37494d655fc476b499cf056f6435518833ae87795aab58744c3c61cc6e2d35e8
1acc31e468ee9ff2d6601bea2d2eb10c464508bb7150073479303b3753dd92b4
O=C(CN1CCC(n2c(=O)[nH]c3ccccc32)CC1)N[C@H]1CCc2ccccc2[C@H]1Cc1cccnc1
O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[#7:4].[#7;a:5]:[c:6]:[c:7]-[C:8]-[CH;D3;+0:9]1-[CH;D3;+0:10](-[NH2;D1;+0:11])-[C:12]-[C:13]-[c:14]:[c:15]-1:[c:16]>>[#7:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:11]-[C@H;D3;+0:10]1-[C:12]-[C:13]-[c:14]:[c:15](:[c:16])-[C@H;D3;+0:9]-1-[C:8]-[c:7]:[c:6]:[#7;a:5]
22
[{"value": 22.0, "product": null, "details": "PERCENTYIELD", "is_desired": false}]
100
CELSIUS
18
HOUR
A solution of 2-(1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (HBTU) (0.974 g, 2.57 mmol), 4-(2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-1-piperidineacetic acid (1.20 g, 2.57 mmol), and N,N-diisopropylethylamine (1.8 mL, 10.3 mmol) in N,N-dimethylformamide (15 mL) was stirred at room temperature f...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Primary amine
Secondary amide
null
null
c1ccc2c(c1)CCCC2.C1CC[NH]CC1.c1ccc2[nH]cnc2c1.c1ccncc1
HO-
CN(C=O)C
100
18
COc1ccc2c(c1)CCC(N)C2Cc1cccnc1.Cl.O=C(O)CN1CCC(n2c(=O)[nH]c3ccccc32)CC1>CN(C=O)C>COc1ccc2c(c1)CC[C@H](NC(=O)CN1CCC(n3c(=O)[nH]c4ccccc43)CC1)[C@@H]2Cc1cccnc1.Cl
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-228917398cef42f3a34830673e83d2fe
COc1ccc2c(c1)CC[C@H](NC(=O)CN1CCC(n3c(=O)[nH]c4ccccc43)CC1)[C@@H]2Cc1cccnc1.Cl>>Cl.O=C(CN1CCC(n2c(=O)[nH]c3ccccc32)CC1)N[C@H]1CCc2cc(O)ccc2[C@H]1Cc1cccnc1
CO.Cl.Cl.O=C1NC2=C(N1C1CCN(CC1)CC(=O)N[C@@H]1[C@@H](C3=CC=C(C=C3CC1)OC)CC=1C=NC=CC1)C=CC=C2.B(Br)(Br)Br>>Cl.Cl.O=C1NC2=C(N1C1CCN(CC1)CC(=O)N[C@@H]1[C@@H](C3=CC=C(C=C3CC1)O)CC=1C=NC=CC1)C=CC=C2
C[O:29][c:28]1[cH:27][c:26]2[c:32]([cH:31][cH:30]1)[C@@H:33]([CH2:34][c:35]1[cH:36][cH:37][cH:38][n:39][cH:40]1)[C@@H:23]([NH:22][C:4](=[O:3])[CH2:5][N:6]1[CH2:7][CH2:8][CH:9]([n:10]3[c:11](=[O:12])[nH:13][c:14]4[cH:15][cH:16][cH:17][cH:18][c:19]34)[CH2:20][CH2:21]1)[CH2:24][CH2:25]2.[ClH:1]>>[ClH:1].[O:3]=[C:4]([CH2:5...
COc1ccc2c(c1)CC[C@H](NC(=O)CN1CCC(n3c(=O)[nH]c4ccccc43)CC1)[C@@H]2Cc1cccnc1.Cl
Cl.O=C(CN1CCC(n2c(=O)[nH]c3ccccc32)CC1)N[C@H]1CCc2cc(O)ccc2[C@H]1Cc1cccnc1
null
null
ClCCl
Miscellaneous
OtherReaction
005318874c4792a3ed14897fb19099f1f6e548b285f476e19a15213a92356c2d
0bab01685da92cdead9c84b3a9c513c0e9bd4114585991beae2460d8c47b3623
O=C(CN1CCC(n2c(=O)[nH]c3ccccc32)CC1)N[C@H]1CCc2ccccc2[C@H]1Cc1cccnc1
C-[O;H0;D2;+0:1]-[c:2](:[c:3]):[c:4]>>[OH;D1;+0:1]-[c:2](:[c:3]):[c:4]
68
[{"value": 68.0, "product": "Cl.Cl.O=C1NC2=C(N1C1CCN(CC1)CC(=O)N[C@@H]1[C@@H](C3=CC=C(C=C3CC1)O)CC=1C=NC=CC1)C=CC=C2", "details": "PERCENTYIELD", "is_desired": false}]
null
null
0.5
HOUR
A solution of 4-(2,3-dihydro-2-oxo-1H-benzimidazol-1-yl)-N-[cis-1,2,3,4-tetrahydro-6-methoxy-1-(3-pyridinylmethyl)-2-naphthalenyl]-1-piperidineacetamide 19 (0.28 g, 0.37 mmol) in dichloromethane (2 mL) was added dropwise to a solution of boron tribromide (1.8 mmol) in dichloromethane (22 mL) at 0° C. After stirring the...
10.6084/m9.figshare.5104873.v1
null
Ether
Aromatic alcohol
null
null
C1CC[NH]CC1.c1ccc2[nH]cnc2c1.c1ccc2c(c1)CCCC2.c1ccncc1
Other
ClCCl
null
0.5
COc1ccc2c(c1)CC[C@H](NC(=O)CN1CCC(n3c(=O)[nH]c4ccccc43)CC1)[C@@H]2Cc1cccnc1.Cl>ClCCl>Cl.O=C(CN1CCC(n2c(=O)[nH]c3ccccc32)CC1)N[C@H]1CCc2cc(O)ccc2[C@H]1Cc1cccnc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-4ba49e669c8944568145ff09ba5e9264
CC(=O)Cc1ccncc1>>C=CC(=O)Cc1cccnc1
N1=CC=C(C=C1)CC(C)=O.FC=1C=C(C=O)C=CC1OC.N1CCCCC1>>N1=CC(=CC=C1)CC(C=C)=O
[CH3:2][C:3](=[O:4])[CH2:5][c:6]1[cH:7][cH:8][n:10][cH:9][cH:11]1>>[CH2:1]=[CH:2][C:3](=[O:4])[CH2:5][c:6]1[cH:7][cH:8][cH:9][n:10][cH:11]1
CC(=O)Cc1ccncc1
C=CC(=O)Cc1cccnc1
null
null
C1(=CC=CC=C1)C
Miscellaneous
OtherReaction
58ac067248252835f00a3165c674651cacbcbd5887568465d5bc1f845a3f9fd5
a4ea716c40716a0b7f0a729baa69598349e4dc3a183004a01a28b0d16986acd9
c1ccncc1
[CH3;D1;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[c:5]1:[c:6]:[cH;D2;+0:7]:[n;H0;D2;+0:8]:[cH;D2;+0:9]:[cH;D2;+0:10]:1>>[C;D1;H2:11]=[CH;D2;+0:1]-[C:2](=[O;D1;H0:3])-[C:4]-[c:5]1:[c:6]:[cH;D2;+0:7]:[cH;D2;+0:9]:[n;H0;D2;+0:8]:[cH;D2;+0:10]:1
146.9
[{"value": 80.0, "product": "N1=CC(=CC=C1)CC(C=C)=O", "details": "PERCENTYIELD", "is_desired": false}, {"value": 146.9, "product": "N1=CC(=CC=C1)CC(C=C)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
18
HOUR
A solution of 4-pyridylacetone (1.0 g, 7.4 mmol), 3-fluoro-p-anisaldehyde (1.25 g, 8.1 mmol), and piperidine (0.13 g, 1.5 mmol) in toluene (50 ml) was heated to reflux. After 18 hours, the reaction was cooled to room temperature and the solvent was removed under reduced pressure. The crude product (3.0 g) was purified ...
10.6084/m9.figshare.5104873.v1
null
Ketone
Ketone.Vinyl
c1ccncc1
c1ccncc1
c1ccncc1
Other
C1(=CC=CC=C1)C
null
18
CC(=O)Cc1ccncc1>C1(=CC=CC=C1)C>C=CC(=O)Cc1cccnc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ede2249cb08b4a579ea218c9296d4d94
CC(=O)Cc1ccncc1.O=Cc1ccccc1>>CC(=O)C(=Cc1ccccc1)c1ccncc1
N1=CC=C(C=C1)CC(C)=O.C(C1=CC=CC=C1)=O.N1CCCCC1>>C1(=CC=CC=C1)C=C(C(C)=O)C1=CC=NC=C1
[CH3:1][C:2](=[O:3])[CH2:4][c:12]1[cH:13][cH:14][n:15][cH:16][cH:17]1.O=[CH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1>>[CH3:1][C:2](=[O:3])[C:4](=[CH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1)[c:12]1[cH:13][cH:14][n:15][cH:16][cH:17]1
CC(=O)Cc1ccncc1.O=Cc1ccccc1
CC(=O)C(=Cc1ccccc1)c1ccncc1
null
null
C1=CC=CC=C1
C-C Coupling
Aldol condensation
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
C(=Cc1ccncc1)c1ccccc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C;D1;H3:5]-[C:6](=[O;D1;H0:7])-[CH2;D2;+0:8]-[c:9]1:[c:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1>>[C;D1;H3:5]-[C:6](=[O;D1;H0:7])-[C;H0;D3;+0:8](=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[c:9]1:[c:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1
78.7
[{"value": 78.0, "product": "C1(=CC=CC=C1)C=C(C(C)=O)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 78.7, "product": "C1(=CC=CC=C1)C=C(C(C)=O)C1=CC=NC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example A-1, step 1, 4-pyridylacetone (step 1) (1 g, 7.4 mmol) was condensed with benzaldehyde (790 mg, 7.4 mmol) in benzene (15 mL) containing piperidine (50 mg) at reflux. The desired 4-phenyl-3-(4-pyridyl)-3-butene-2-one (1.3 g, 78%) was obtained as a crystalline solid: m. p. 101-103° C. Anal....
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
c1ccccc1.c1ccncc1
HO-
C1=CC=CC=C1
null
null
CC(=O)Cc1ccncc1.O=Cc1ccccc1>C1=CC=CC=C1>CC(=O)C(=Cc1ccccc1)c1ccncc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f58e317b4f9744969269814759558a45
CC(=O)C(=Cc1ccccc1)c1ccncc1.OO>>CC(=O)C1(c2ccncc2)OC1c1ccccc1
C1(=CC=CC=C1)C=C(C(C)=O)C1=CC=NC=C1.OO.[OH-].[Na+]>>C1(=CC=CC=C1)C1C(C(C)=O)(O1)C1=CC=NC=C1
[CH3:1][C:2](=[O:3])[C:4]([c:5]1[cH:6][cH:7][n:8][cH:9][cH:10]1)=[CH:12][c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1.O[OH:11]>>[CH3:1][C:2](=[O:3])[C:4]1([c:5]2[cH:6][cH:7][n:8][cH:9][cH:10]2)[O:11][CH:12]1[c:13]1[cH:14][cH:15][cH:16][cH:17][cH:18]1
CC(=O)C(=Cc1ccccc1)c1ccncc1.OO
CC(=O)C1(c2ccncc2)OC1c1ccccc1
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
5310d49b11c467cc6f2bb1b67ae31fe7fbc0be3f375d7a005d31b2362cbddf0d
7ff20700d82072065bf203f7a44745e56ef236256026869b544d4eff6bac8783
c1ccc(C2OC2c2ccncc2)cc1
O-[OH;D1;+0:1].[C;D1;H3:2]-[C:3](=[O;D1;H0:4])-[C;H0;D3;+0:5](=[CH;D2;+0:6]-[c:7](:[c:8]):[c:9])-[c:10]1:[c:11]:[c:12]:[#7;a:13]:[c:14]:[c:15]:1>>[C;D1;H3:2]-[C:3](=[O;D1;H0:4])-[C;H0;D4;+0:5]1(-[c:10]2:[c:11]:[c:12]:[#7;a:13]:[c:14]:[c:15]:2)-[O;H0;D2;+0:1]-[CH;D3;+0:6]-1-[c:7](:[c:8]):[c:9]
20
[{"value": 20.0, "product": "C1(=CC=CC=C1)C1C(C(C)=O)(O1)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example A-1, step 2, a solution of 4-phenyl-3-(4-pyridyl)-3-butene-2-one (step 2) (1.25 g, 5.6 mmol) in methanol (20 ml) was treated with 30% aqueous hydrogen peroxide (1 ml) in the presence of sodium hydroxide (230 mg, 5.7 mmol). The crude product was purified by chromatography (silica gel, 1:1 ...
10.6084/m9.figshare.5104873.v1
null
Ketone.Peroxide
Ketone.Ether
null
C1CO1
c1ccncc1.C1CO1.c1ccccc1
HO-
CO
null
null
CC(=O)C(=Cc1ccccc1)c1ccncc1.OO>CO>CC(=O)C1(c2ccncc2)OC1c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-69b96eedf34c4a37acb566602bfb5210
CC(=O)C1(c2ccncc2)OC1c1ccccc1.NN>>Cc1n[nH]c(-c2ccccc2)c1-c1ccncc1
C1(=CC=CC=C1)C1C(C(C)=O)(O1)C1=CC=NC=C1.NN>>CC1=NNC(=C1C1=CC=NC=C1)C1=CC=CC=C1
O=[C:2]([CH3:1])[C:12]1([c:13]2[cH:14][cH:15][n:16][cH:17][cH:18]2)O[CH:5]1[c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1.[NH2:3][NH2:4]>>[CH3:1][c:2]1[n:3][nH:4][c:5](-[c:6]2[cH:7][cH:8][cH:9][cH:10][cH:11]2)[c:12]1-[c:13]1[cH:14][cH:15][n:16][cH:17][cH:18]1
CC(=O)C1(c2ccncc2)OC1c1ccccc1.NN
Cc1n[nH]c(-c2ccccc2)c1-c1ccncc1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
3d767427471af8679ab96a9ef8b8a5608e72cdf8ed95f8ea7ae504a611c2b5b3
bb1c7e9a3d57170de2c73b6fa3f5bc7c31ad9976d2759941c3ea46738c101a22
c1ccc(-c2[nH]ncc2-c2ccncc2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[C;H0;D4;+0:3]1(-[c;H0;D3;+0:4]2:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:2)-O-[CH;D3;+0:10]-1-[c;H0;D3;+0:11](:[c:12]:[c:13]):[c:14]:[c:15].[NH2;D1;+0:16]-[NH2;D1;+0:17]>>[C;D1;H3:2]-[c;H0;D3;+0:1]1:[n;H0;D2;+0:16]:[nH;D2;+0:17]:[c;H0;D3;+0:10](-[c;H0;D3;+0:11](:[c:12]:[c:13]):[c:14]:[c:15]):[c;...
35
[{"value": 35.0, "product": "CC1=NNC(=C1C1=CC=NC=C1)C1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 34.4, "product": "CC1=NNC(=C1C1=CC=NC=C1)C1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
Using the procedure of Example A-1, step 3, a solution of 4-phenyl-3-(4-pyridyl)-3,4-epoxy-2-butanone (step 3) (250 mg, 1 mmol) in ethanol (15 ml) was treated with anhydrous hydrazine (50 mg, 1.5 mmol) and heated to reflux for 4 hours. The crude product was purified by chromatography (silica gel, 1:1 acetone/hexane). T...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ether
null
C1CO1
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1.c1ccncc1
HO-
C(C)O
null
null
CC(=O)C1(c2ccncc2)OC1c1ccccc1.NN>C(C)O>Cc1n[nH]c(-c2ccccc2)c1-c1ccncc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e6655c96939d4951a24c084af478a9ee
C1CCNCC1.Cc1ccccc1.Cc1ccccc1C=O>>CC(=O)C(=Cc1ccccc1C)c1ccncc1
C1(=CC=CC=C1)C.C=1(C(=CC=CC1)C=O)C.N1CCCCC1.O>>CC1=C(C=CC=C1)C=C(C(C)=O)C1=CC=NC=C1
[CH2:13]1[CH2:14][CH2:15][NH:16][CH2:17][CH2:18]1.c1cc[cH:4][c:2]([CH3:1])c1.[O:3]=[CH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][c:11]1[CH3:12]>>[CH3:1][C:2](=[O:3])[C:4](=[CH:5][c:6]1[cH:7][cH:8][cH:9][cH:10][c:11]1[CH3:12])[c:13]1[cH:14][cH:15][n:16][cH:17][cH:18]1
C1CCNCC1.Cc1ccccc1.Cc1ccccc1C=O
CC(=O)C(=Cc1ccccc1C)c1ccncc1
null
null
null
C-C Coupling
OtherReaction
9e5c85b79e15bdcaaf9e3ec702b4eda0aef404997135a9ecc0a250fe682cf221
c2326e088efe6b686881bcc39eafc3fbffc8a8d1281e2dcdeecdd838d9d42f48
C(=Cc1ccncc1)c1ccccc1
[C;D1;H3:1]-[c;H0;D3;+0:2]1:[cH;D2;+0:3]:c:c:c:c:1.[CH2;D2;+0:4]1-[CH2;D2;+0:5]-[CH2;D2;+0:6]-[NH;D2;+0:7]-[CH2;D2;+0:8]-[CH2;D2;+0:9]-1.[O;H0;D1;+0:10]=[CH;D2;+0:11]-[c:12](:[c:13]):[c:14]>>[C;D1;H3:1]-[C;H0;D3;+0:2](=[O;H0;D1;+0:10])-[C;H0;D3;+0:3](=[CH;D2;+0:11]-[c:12](:[c:13]):[c:14])-[c;H0;D3;+0:4]1:[cH;D2;+0:5]:[...
null
[]
null
null
15
HOUR
A solution of 4-pyrridylacetone (Example A-5, step 1) (0.75 g, 5.56 mmol), o-tolualdehyde (0.73 g, 5.56 mmol) and piperidine (100 mg) in toluene (50 ml) was heated to reflux. Water generated during the reaction was removed by a Dean-Stark trap. After heating at reflux for 5 hours, the reaction mixture was stirred at ro...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Secondary amine
Ketone
C1CCNCC1.c1ccccc1
c1ccncc1
c1ccccc1.c1ccncc1
Other
null
null
15
C1CCNCC1.Cc1ccccc1.Cc1ccccc1C=O>>CC(=O)C(=Cc1ccccc1C)c1ccncc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fcfae01ee9d9406f8c01efe92ac822bc
CC(=O)C(=Cc1ccccc1C)c1ccncc1.OO>>CC(=O)C1(c2ccncc2)OC1c1ccccc1C
CC1=C(C=CC=C1)C=C(C(C)=O)C1=CC=NC=C1.OO.[OH-].[Na+]>>CC1=C(C=CC=C1)C1C(C(C)=O)(O1)C1=CC=NC=C1
[CH3:1][C:2](=[O:3])[C:4]([c:5]1[cH:6][cH:7][n:8][cH:9][cH:10]1)=[CH:12][c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[CH3:19].O[OH:11]>>[CH3:1][C:2](=[O:3])[C:4]1([c:5]2[cH:6][cH:7][n:8][cH:9][cH:10]2)[O:11][CH:12]1[c:13]1[cH:14][cH:15][cH:16][cH:17][c:18]1[CH3:19]
CC(=O)C(=Cc1ccccc1C)c1ccncc1.OO
CC(=O)C1(c2ccncc2)OC1c1ccccc1C
null
null
O.CO
Heteroatom Alkylation and Arylation
OtherReaction
5310d49b11c467cc6f2bb1b67ae31fe7fbc0be3f375d7a005d31b2362cbddf0d
7ff20700d82072065bf203f7a44745e56ef236256026869b544d4eff6bac8783
c1ccc(C2OC2c2ccncc2)cc1
O-[OH;D1;+0:1].[C;D1;H3:2]-[C:3](=[O;D1;H0:4])-[C;H0;D3;+0:5](=[CH;D2;+0:6]-[c:7](:[c:8]):[c:9])-[c:10]1:[c:11]:[c:12]:[#7;a:13]:[c:14]:[c:15]:1>>[C;D1;H3:2]-[C:3](=[O;D1;H0:4])-[C;H0;D4;+0:5]1(-[c:10]2:[c:11]:[c:12]:[#7;a:13]:[c:14]:[c:15]:2)-[O;H0;D2;+0:1]-[CH;D3;+0:6]-1-[c:7](:[c:8]):[c:9]
null
[]
null
null
70
HOUR
To a solution of 4-(2-methylphenyl)-3-(4-pyridyl)-3-butene-2-one (step 1) (1.0 g, 4.2 mmol) in methyl alcohol (18 ml), a solution of H2O2 (30% by wt.) (0.95 g, 8.4 mmol) and sodium hydroxide (0.18 g 4.6 mmol) in water (4 ml) was added. The reaction was stirred at room temperature for 70 hours. After methyl alcohol was ...
10.6084/m9.figshare.5104873.v1
null
Ketone.Peroxide
Ketone.Ether
null
C1CO1
c1ccncc1.C1CO1.c1ccccc1
HO-
O.CO
null
70
CC(=O)C(=Cc1ccccc1C)c1ccncc1.OO>O.CO>CC(=O)C1(c2ccncc2)OC1c1ccccc1C
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8f872610fe0847baa821c66233be02f3
CC(=O)C1(c2ccncc2)OC1c1ccccc1C.NN>>Cc1ccccc1-c1n[nH]c(C)c1-c1ccncc1
CC1=C(C=CC=C1)C1C(C(C)=O)(O1)C1=CC=NC=C1.O.NN>>CC1=C(C(=NN1)C1=C(C=CC=C1)C)C1=CC=NC=C1
O=[C:11]([CH3:12])[C:13]1([c:14]2[cH:15][cH:16][n:17][cH:18][cH:19]2)O[CH:8]1[c:7]1[c:2]([CH3:1])[cH:3][cH:4][cH:5][cH:6]1.[NH2:9][NH2:10]>>[CH3:1][c:2]1[cH:3][cH:4][cH:5][cH:6][c:7]1-[c:8]1[n:9][nH:10][c:11]([CH3:12])[c:13]1-[c:14]1[cH:15][cH:16][n:17][cH:18][cH:19]1
CC(=O)C1(c2ccncc2)OC1c1ccccc1C.NN
Cc1ccccc1-c1n[nH]c(C)c1-c1ccncc1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
3d767427471af8679ab96a9ef8b8a5608e72cdf8ed95f8ea7ae504a611c2b5b3
bb1c7e9a3d57170de2c73b6fa3f5bc7c31ad9976d2759941c3ea46738c101a22
c1ccc(-c2n[nH]cc2-c2ccncc2)cc1
O=[C;H0;D3;+0:1](-[C;D1;H3:2])-[C;H0;D4;+0:3]1(-[c;H0;D3;+0:4]2:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:2)-O-[CH;D3;+0:10]-1-[c;H0;D3;+0:11](:[c:12]:[c:13]):[c:14](-[C;D1;H3:15]):[c:16].[NH2;D1;+0:17]-[NH2;D1;+0:18]>>[C;D1;H3:2]-[c;H0;D3;+0:1]1:[nH;D2;+0:17]:[n;H0;D2;+0:18]:[c;H0;D3;+0:10](-[c;H0;D3;+0:11](:[c:12]:[c:13]):[c:...
null
[]
null
null
null
null
A solution of 4-(2-methylphenyl)-3-(4-pyridyl)-3,4-epoxy-2-butanone (step 2) (0.11 g, 0.434 mmol) and hydrazine hydrate (0.043 g, 0.868 mmol) in ethyl alcohol (50 ml) was heated at reflux for 20 hours. The solvent was removed and the resulting residue was purified by chromatography to give 4-[5-methyl-3-(2-methylphenyl...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ether
null
C1CO1
c1cn[nH]c1
c1ccccc1.c1cn[nH]c1.c1ccncc1
HO-
C(C)O
null
null
CC(=O)C1(c2ccncc2)OC1c1ccccc1C.NN>C(C)O>Cc1ccccc1-c1n[nH]c(C)c1-c1ccncc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6bc658d1bfb6474e966703232df05d6f
CC(C)(C)[Si](C)(C)Cl.OCCNN=C(Cc1ccncc1)c1ccc(F)cc1>>CC(C)(C)[Si](C)(C)OCCNN=C(Cc1ccncc1)c1ccc(F)cc1
O.OCCNN=C(CC1=CC=NC=C1)C1=CC=C(C=C1)F.CC(C)(C)[Si](C)(C)Cl.N1C=NC=C1>>CC(C)(C)[Si](OCCNN=C(CC1=CC=NC=C1)C1=CC=C(C=C1)F)(C)C
Cl[Si:5]([C:2]([CH3:1])([CH3:3])[CH3:4])([CH3:6])[CH3:7].[OH:8][CH2:9][CH2:10][NH:11][N:12]=[C:13]([CH2:14][c:15]1[cH:16][cH:17][n:18][cH:19][cH:20]1)[c:21]1[cH:22][cH:23][c:24]([F:25])[cH:26][cH:27]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([CH3:6])([CH3:7])[O:8][CH2:9][CH2:10][NH:11][N:12]=[C:13]([CH2:14][c:15]1[cH:16][...
CC(C)(C)[Si](C)(C)Cl.OCCNN=C(Cc1ccncc1)c1ccc(F)cc1
CC(C)(C)[Si](C)(C)OCCNN=C(Cc1ccncc1)c1ccc(F)cc1
null
null
CN(C)C=O
Protection
Alcohol protection with silyl ethers
0085cd6629412592263fdf1537bdf8c19ef10dbeafe6f880807464d8107fa715
d2a170d01b2f3ec57d6fac058519475050ba5531f5d304635fb42e153d5bb9b5
N=C(Cc1ccncc1)c1ccccc1
Cl-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7].[C:8]-[C:9]-[OH;D1;+0:10]>>[C:8]-[C:9]-[O;H0;D2;+0:10]-[Si;H0;D4;+0:1](-[C;D1;H3:2])(-[C;D1;H3:3])-[C:4](-[C;D1;H3:5])(-[C;D1;H3:6])-[C;D1;H3:7]
98
[{"value": 98.0, "product": "CC(C)(C)[Si](OCCNN=C(CC1=CC=NC=C1)C1=CC=C(C=C1)F)(C)C", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a solution of the 1-(4-fluorophenyl)-2-(4-pyridinyl)ethanone (2-hydroxyethyl)hydrazone prepared in step 1 (2.73 g, 0.01 mol) and (1,1-dimethylethyl)dimethylsilyl chloride (1.5 g, 0.01 mol) in 25 mL of DMF was added imidazole portionwise. The reaction mixture was stirred at room temperature overnight. Water was added...
10.6084/m9.figshare.5104873.v1
null
Primary alcohol.Silyl protective group
TMS ether protective group
null
null
c1ccncc1.c1ccccc1
HCl
CN(C)C=O
null
8
CC(C)(C)[Si](C)(C)Cl.OCCNN=C(Cc1ccncc1)c1ccc(F)cc1>CN(C)C=O>CC(C)(C)[Si](C)(C)OCCNN=C(Cc1ccncc1)c1ccc(F)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b730e5b337614438b0df825449c44415
CC(C)(C)[Si](C)(C)OCCNN=C(Cc1ccncc1)c1ccc(F)cc1.COC(=O)C1CC1.C[Si](C)(C)[N-][Si](C)(C)C>>CC(C)(C)[Si](C)(C)OCCn1nc(-c2ccccc2)c(-c2ccccc2)c1C1CC1
O.C[Si]([N-][Si](C)(C)C)(C)C.[Na+].CC(C)(C)[Si](OCCNN=C(CC1=CC=NC=C1)C1=CC=C(C=C1)F)(C)C.C1(CC1)C(=O)OC>>C1(CC1)C1=C(C(=NN1CCO[Si](C)(C)C(C)(C)C)C1=CC=CC=C1)C1=CC=CC=C1
F[c:17]1[cH:16][cH:15][c:14]([C:13](=[N:12][NH:11][CH2:10][CH2:9][O:8][Si:5]([C:2]([CH3:1])([CH3:3])[CH3:4])([CH3:6])[CH3:7])[CH2:20][c:21]2[cH:22][cH:23]n[cH:25][cH:26]2)[cH:19][cH:18]1.CO[C:27](=O)[CH:28]1[CH2:29][CH2:30]1.C[Si](C)(C)[N-][Si](C)(C)[CH3:24]>>[CH3:1][C:2]([CH3:3])([CH3:4])[Si:5]([CH3:6])([CH3:7])[O:8][...
CC(C)(C)[Si](C)(C)OCCNN=C(Cc1ccncc1)c1ccc(F)cc1.COC(=O)C1CC1.C[Si](C)(C)[N-][Si](C)(C)C
CC(C)(C)[Si](C)(C)OCCn1nc(-c2ccccc2)c(-c2ccccc2)c1C1CC1
null
null
C1CCOC1
Aromatic Heterocycle Formation
OtherReaction
a79510dbe8d2b107583dd2a869abb0ef04cea09d18876fd92cedec7cce043db7
e9e76a09cea9281459d2ce0878168c17feadc9adf5b8840167b7710e55849787
c1ccc(-c2n[nH]c(C3CC3)c2-c2ccccc2)cc1
C-O-[C;H0;D3;+0:1](=O)-[C:2]1-[C:3]-[C:4]-1.C-[Si](-C)(-C)-[N-]-[Si](-C)(-C)-[CH3;D1;+0:5].F-[c;H0;D3;+0:6]1:[c:7]:[c:8]:[c;H0;D3;+0:9](-[C;H0;D3;+0:10](-[CH2;D2;+0:11]-[c;H0;D3;+0:12]2:[c:13]:[cH;D2;+0:14]:n:[cH;D2;+0:15]:[c:16]:2)=[N;H0;D2;+0:17]-[NH;D2;+0:18]-[C:19]-[C:20]):[c:21]:[c:22]:1>>[C:20]-[C:19]-[n;H0;D3;+0...
null
[]
null
null
30
MINUTE
To a solution of sodium hexamethyldisilazide (4.2 mL, 1.0 M in THF) at 0° C. was added a solution of the compound prepared in step 2 (0.78 g, 0.002 mol) in 10 mL of dry THF dropwise. The dark brown solution was stirred at this temperature for 30 minutes. Then a solution of methyl cyclopropanecarboxylate (0.27 g, 0.0026...
10.6084/m9.figshare.5104873.v1
null
Hydrazone.Aromatic halide.Ester.Silyl protective group.Silyl protective group
null
c1ccccc1.c1ccncc1
c1cn[nH]c1.c1ccccc1.c1ccccc1
c1cn[nH]c1.c1ccccc1.c1ccccc1.C1CC1
HF
C1CCOC1
null
0.5
CC(C)(C)[Si](C)(C)OCCNN=C(Cc1ccncc1)c1ccc(F)cc1.COC(=O)C1CC1.C[Si](C)(C)[N-][Si](C)(C)C>C1CCOC1>CC(C)(C)[Si](C)(C)OCCn1nc(-c2ccccc2)c(-c2ccccc2)c1C1CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c37dc49a47b5484cafb5f39fa2a2c164
CCOC(=O)C1CC1c1c(-c2ccncc2)c(-c2ccc(F)cc2)nn1CCO>>O=C(O)C1CC1c1c(-c2ccncc2)c(-c2ccc(F)cc2)nn1CCO
[OH-].[Na+].FC1=CC=C(C=C1)C1=NN(C(=C1C1=CC=NC=C1)C1C(C1)C(=O)OCC)CCO.C1CCC(C1)NC2=NN=C(C3=CC(=C(C=C32)Cl)Cl)C4=CC=NC=C4>>FC1=CC=C(C=C1)C1=NN(C(=C1C1=CC=NC=C1)C1C(C1)C(=O)O)CCO
CC[O:3][C:2](=[O:1])[CH:4]1[CH2:5][CH:6]1[c:7]1[c:8](-[c:9]2[cH:10][cH:11][n:12][cH:13][cH:14]2)[c:15](-[c:16]2[cH:17][cH:18][c:19]([F:20])[cH:21][cH:22]2)[n:23][n:24]1[CH2:25][CH2:26][OH:27]>>[O:1]=[C:2]([OH:3])[CH:4]1[CH2:5][CH:6]1[c:7]1[c:8](-[c:9]2[cH:10][cH:11][n:12][cH:13][cH:14]2)[c:15](-[c:16]2[cH:17][cH:18][c:...
CCOC(=O)C1CC1c1c(-c2ccncc2)c(-c2ccc(F)cc2)nn1CCO
O=C(O)C1CC1c1c(-c2ccncc2)c(-c2ccc(F)cc2)nn1CCO
null
null
O.CO
Deprotection
Ester saponification (alkyl deprotection)
d872e08ad5c85a4add6cd04e6e987e73fead5f79b3f30ba61a81ba5029b29894
38ae1ee78433b9acfb0390501446149c80f88f23ac2d84c60b3369bdab75cec9
c1ccc(-c2n[nH]c(C3CC3)c2-c2ccncc2)cc1
C-C-[O;H0;D2;+0:1]-[C:2](-[C:3])=[O;D1;H0:4]>>[C:3]-[C:2](=[O;D1;H0:4])-[OH;D1;+0:1]
null
[]
null
null
null
null
To a solution of ethyl 2-[3-(4-fluorophenyl)-1-(2-hydroxyethyl)-4-(4-pyridinyl)-1H-pyrazol-5-yl]cyclopropanecarboxylate prepared in accordance with Example A-196 (0.21 g, 0.00045 mol) in 10 mL of methanol was added a solution of sodium hydroxide (0.09 g, 0.0022 mol) in 2 mL of water. The reaction mixture was stirred at...
10.6084/m9.figshare.5104873.v1
null
Ester
Carboxylic acid
null
null
C1CC1.c1ccncc1.c1ccccc1.c1cn[nH]c1
Other
O.CO
null
null
CCOC(=O)C1CC1c1c(-c2ccncc2)c(-c2ccc(F)cc2)nn1CCO>O.CO>O=C(O)C1CC1c1c(-c2ccncc2)c(-c2ccc(F)cc2)nn1CCO
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e4e13147fc66491b8f6fcad33de9cd9b
CN(C)C=O.COC(=O)c1c[nH]cn1.C[Si](C)(C)CCOCCl>>COC(=O)c1ccn(COCC[Si](C)(C)C)c1
[H-].[Na+].CN(C)C=O.N1C=NC(=C1)C(=O)OC.C[Si](C)(C)CCOCCl>>C[Si](CCOCN1C=C(C=C1)C(=O)OC)(C)C
CN(C=O)[CH3:6].n1[c:5]([C:3]([O:2][CH3:1])=[O:4])[cH:17][nH:8][cH:7]1.Cl[CH2:9][O:10][CH2:11][CH2:12][Si:13]([CH3:14])([CH3:15])[CH3:16]>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][cH:7][n:8]([CH2:9][O:10][CH2:11][CH2:12][Si:13]([CH3:14])([CH3:15])[CH3:16])[cH:17]1
CN(C)C=O.COC(=O)c1c[nH]cn1.C[Si](C)(C)CCOCCl
COC(=O)c1ccn(COCC[Si](C)(C)C)c1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
7c5e42e4ce8d87d0453b8cd9567e04cd94c920799410915227b31c72d98ffa60
2984e97dc99d59f23dc9b7338b3c1cfa8c682d0ec9c881b8c684e99fe044da2a
c1cc[nH]c1
C-N(-[CH3;D1;+0:1])-C=O.Cl-[CH2;D2;+0:2]-[#8:3]-[C:4].[C;D1;H3:5]-[#8:6]-[C:7](=[O;D1;H0:8])-[c;H0;D3;+0:9]1:[c:10]:[nH;D2;+0:11]:[cH;D2;+0:12]:n:1>>[C:4]-[#8:3]-[CH2;D2;+0:2]-[n;H0;D3;+0:11]1:[c:10]:[c;H0;D3;+0:9](-[C:7](=[O;D1;H0:8])-[#8:6]-[C;D1;H3:5]):[cH;D2;+0:1]:[cH;D2;+0:12]:1
null
[]
null
null
0.5
HOUR
To a suspension of sodium hydride (1.0 g, 0.025 mol) in 50 mL of DMF was added methyl 4-imidazolecarboxylate (2.95 g, 0.023 mol) portionwise at room temperature. The mixture was stirred at room temperature for 0.5 hours. Then SEM-CL (4.17 g, 0.025 mol) was added dropwise over 5 minutes. The reaction mixture was stirred...
10.6084/m9.figshare.5104873.v1
null
Primary halide.Ester.Ether.Tertiary amide
Ester.Ether
c1c[nH]cn1
c1cc[nH]c1
c1cc[nH]c1
HCl
null
null
0.5
CN(C)C=O.COC(=O)c1c[nH]cn1.C[Si](C)(C)CCOCCl>>COC(=O)c1ccn(COCC[Si](C)(C)C)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-fb50f6cfbe3d4f45adc3c70edc36c9b3
Cc1[nH]nc(-c2ccc(F)cc2)c1-c1ccncc1.[O]=[Mn](=[O])(=[O])[O-].[O]=[Mn](=[O])(=[O])[O-]>>O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
O.FC1=CC=C(C=C1)C1=NNC(=C1C1=CC=NC=C1)C.[Mn](=O)(=O)(=O)[O-].[K+].[Mn](=O)(=O)(=O)[O-].[K+]>>FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)O)C1=CC=NC=C1
[CH3:2][c:4]1[nH:5][n:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([F:12])[cH:13][cH:14]2)[c:15]1-[c:16]1[cH:17][cH:18][n:19][cH:20][cH:21]1.[O]=[Mn](=[O])(=[O])[O-:3].[O]=[Mn](=[O])([O-])=[O:1]>>[O:1]=[C:2]([OH:3])[c:4]1[n:5][nH:6][c:7](-[c:8]2[cH:9][cH:10][c:11]([F:12])[cH:13][cH:14]2)[c:15]1-[c:16]1[cH:17][cH:18][n:19][cH:20]...
Cc1[nH]nc(-c2ccc(F)cc2)c1-c1ccncc1.[O]=[Mn](=[O])(=[O])[O-].[O]=[Mn](=[O])(=[O])[O-]
O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
null
null
C(C)(C)(C)O
Acylation
OtherReaction
7769a4cd09a67e270ac2d1d32df6b7a59b468ff590f9c59723b72ba3c8deb342
903e48d04e4504a4fe6977f5e5582144adff237d0488a4542a1907161cf0134c
c1ccc(-c2[nH]ncc2-c2ccncc2)cc1
[CH3;D1;+0:1]-[c:2]1:[c:3]:[c:4](-[c:5]):[n;H0;D2;+0:6]:[nH;D2;+0:7]:1.[O-;H0;D1:8]-[Mn](=[O])(=[O])=[O].[O-]-[Mn](=[O;H0;D1;+0:9])(=[O])=[O]>>[O;H0;D1;+0:9]=[C;H0;D3;+0:1](-[OH;D1;+0:8])-[c:2]1:[c:3]:[c:4](-[c:5]):[nH;D2;+0:6]:[n;H0;D2;+0:7]:1
null
[]
null
null
8
HOUR
A mixture of 4-[3-(4-fluorophenyl)-5-methyl-1H-pyrazol-4-yl]pyridine prepared as set forth in Example A-4 (5.83 g, 24.0909 mmol) and potassium permanganate (7.6916 g, 48.1818 mmol) in water (7.5 ml) and tert-butanol (10 ml) was heated at reflux for 6 hours (or until all the potassium permanganate was consumed). The mix...
10.6084/m9.figshare.5104873.v1
null
null
Carboxylic acid
null
null
c1cn[nH]c1.c1ccccc1.c1ccncc1
HO-
C(C)(C)(C)O
null
8
Cc1[nH]nc(-c2ccc(F)cc2)c1-c1ccncc1.[O]=[Mn](=[O])(=[O])[O-].[O]=[Mn](=[O])(=[O])[O-]>C(C)(C)(C)O>O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1cc31954fc634c00a423cc1613ed9fd0
O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1>>OCc1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
[H-].[Al+3].[Li+].[H-].[H-].[H-].O.FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)O)C1=CC=NC=C1.[OH-].[K+].[H-].[Al+3].[Li+].[H-].[H-].[H-]>>FC1=CC=C(C=C1)C1=C(C(=NN1)CO)C1=CC=NC=C1
O=[C:2]([OH:1])[c:3]1[n:4][nH:5][c:6](-[c:7]2[cH:8][cH:9][c:10]([F:11])[cH:12][cH:13]2)[c:14]1-[c:15]1[cH:16][cH:17][n:18][cH:19][cH:20]1>>[OH:1][CH2:2][c:3]1[n:4][nH:5][c:6](-[c:7]2[cH:8][cH:9][c:10]([F:11])[cH:12][cH:13]2)[c:14]1-[c:15]1[cH:16][cH:17][n:18][cH:19][cH:20]1
O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
OCc1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
null
null
O.C1CCOC1
Reduction
Reduction of carboxylic acid to primary alcohol
0db83a5ebe1e318b78b55461cf7eb8f7c004eef0f9e3b6666d3df4c96b5f665e
93b4621647b04d2ad2f2825215b1567f171ba61fe10d136b5db6ea0470aa4932
c1ccc(-c2[nH]ncc2-c2ccncc2)cc1
O=[C;H0;D3;+0:1](-[O;D1;H1:2])-[c:3]1:[#7;a:4]:[#7;a:5]:[c:6]:[c:7]:1>>[O;D1;H1:2]-[CH2;D2;+0:1]-[c:3]1:[#7;a:4]:[#7;a:5]:[c:6]:[c:7]:1
56.5
[{"value": 56.5, "product": "FC1=CC=C(C=C1)C1=C(C(=NN1)CO)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
To a suspension of 5-(4-fluorophenyl)-4-(4-pyridinyl)-1H-pyrazole-3-carboxylic acid, monohydrate prepared in accordance with Example A-200 (0.526 g, 2.0 mmol) in dry THF (15 ml) at reflux under nitrogen, a solution of 1N lithium aluminum hydride in THF (4.0 ml, 4.0 mmol) was added dropwise over 15 minutes. A precipitat...
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid
Primary alcohol
null
null
c1cn[nH]c1.c1ccccc1.c1ccncc1
Other
O.C1CCOC1
null
null
O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1>O.C1CCOC1>OCc1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f36b5071028046928e6e1687e3cb3bc8
CCCCOC(=O)N1CCNCC1.CN(C)C=O.O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1>>CC(C)(C)OC(=O)N1CCN(C(=O)c2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1
C(CCC)OC(=O)N1CCNCC1.CN1CCOCC1.O.FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)O)C1=CC=NC=C1.ON1N=NC2=C1C=CC=C2.CN(C)C=O>>FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)N1CCN(CC1)C(=O)OC(C)(C)C)C1=CC=NC=C1
C([CH3:1])[CH2:4][CH2:2][O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][NH:11][CH2:32][CH2:33]1.CN(C=O)[CH3:3].O[C:12](=[O:13])[c:14]1[n:15][nH:16][c:17](-[c:18]2[cH:19][cH:20][c:21]([F:22])[cH:23][cH:24]2)[c:25]1-[c:26]1[cH:27][cH:28][n:29][cH:30][cH:31]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][...
CCCCOC(=O)N1CCNCC1.CN(C)C=O.O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
CC(C)(C)OC(=O)N1CCN(C(=O)c2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1
null
null
C(C)(=O)OCC
Acylation
OtherReaction
c909fd92dae84461bd7f8e029068785c25084aa8358fc8856c619817f749d07a
96600684aa7d168a6aca35abaa2f4fdb56ee5830af274f4369f6150052490b6e
O=C(c1n[nH]c(-c2ccccc2)c1-c1ccncc1)N1CCNCC1
C-N(-[CH3;D1;+0:1])-C=O.O-[C;H0;D3;+0:2](=[O;D1;H0:3])-[c:4]1:[#7;a:5]:[#7;a:6]:[c:7]:[c:8]:1.[CH3;D1;+0:9]-C-[CH2;D2;+0:10]-[CH2;D2;+0:11]-[#8:12]-[C:13](=[O;D1;H0:14])-[#7:15]1-[C:16]-[C:17]-[NH;D2;+0:18]-[C:19]-[C:20]-1>>[CH3;D1;+0:9]-[C;H0;D4;+0:11](-[CH3;D1;+0:1])(-[CH3;D1;+0:10])-[#8:12]-[C:13](=[O;D1;H0:14])-[#7...
78.4
[{"value": 78.4, "product": "FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)N1CCN(CC1)C(=O)OC(C)(C)C)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
0
CELSIUS
1
HOUR
To a solution of 5-(4-fluorophenyl)-4-(4-pyridinyl)-1H-pyrazole-3-carboxylic acid, monohydrate prepared in accordance with Example A-200 (0.9905 g, 3.5 mmol) and 1-hydroxybenzotriazole (0.4824 g, 3.57 mmol) in DMF (20 ml) at 0° C. under nitrogen, 1-(3-dimethylaminopropyl)3-ethylcarbodiiminde hydrochloride (0.6984 g, 3....
10.6084/m9.figshare.5104873.v1
null
Carboxylic acid.Ether.Tertiary amide.Secondary amine
Ether.Tertiary amide.Boc
C1C[NH]CCN1
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1cn[nH]c1.c1ccccc1.c1ccncc1
HO-
C(C)(=O)OCC
0
1
CCCCOC(=O)N1CCNCC1.CN(C)C=O.O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1>C(C)(=O)OCC>CC(C)(C)OC(=O)N1CCN(C(=O)c2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-42d6b0052f2c4a7aa5b1572e7f3072a3
BrBr.Cn1cc(-c2ccncc2)c(-c2ccc(F)cc2)n1>>Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1Br
FC1=CC=C(C=C1)C1=NN(C=C1C1=CC=NC=C1)C.BrBr>>BrC1=C(C(=NN1C)C1=CC=C(C=C1)F)C1=CC=NC=C1
Br[Br:20].[CH3:1][n:2]1[n:3][c:4](-[c:5]2[cH:6][cH:7][c:8]([F:9])[cH:10][cH:11]2)[c:12](-[c:13]2[cH:14][cH:15][n:16][cH:17][cH:18]2)[cH:19]1>>[CH3:1][n:2]1[n:3][c:4](-[c:5]2[cH:6][cH:7][c:8]([F:9])[cH:10][cH:11]2)[c:12](-[c:13]2[cH:14][cH:15][n:16][cH:17][cH:18]2)[c:19]1[Br:20]
BrBr.Cn1cc(-c2ccncc2)c(-c2ccc(F)cc2)n1
Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1Br
null
null
C(C)(=O)O.CN(C)C=O
Functional Group Interconversion
Bromination
62bd82ea16bda9045775280a9a6f541acc1cff475707d068db9b03a630cda50f
3c4065ab4a8681675e06a527dcad54d701c7bfdcac9f73f87773b05034108934
c1ccc(-c2n[nH]cc2-c2ccncc2)cc1
Br-[Br;H0;D1;+0:1].[C;D1;H3:2]-[#7;a:3]1:[#7;a:4]:[c:5](-[c:6]):[c:7](-[c:8]):[cH;D2;+0:9]:1>>[Br;H0;D1;+0:1]-[c;H0;D3;+0:9]1:[#7;a:3](-[C;D1;H3:2]):[#7;a:4]:[c:5](-[c:6]):[c:7]:1-[c:8]
35
[{"value": 35.0, "product": "BrC1=C(C(=NN1C)C1=CC=C(C=C1)F)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 35.0, "product": "BrC1=C(C(=NN1C)C1=CC=C(C=C1)F)C1=CC=NC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
60
CELSIUS
null
null
To a solution of 4-[3-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]pyridine (2.7 g, 10.67 mmol) (prepared in accordance with Example A-212) in acetic acid (30 mL) and DMF (13 mL) was added bromine (19.5 g, 122.0 mmol). The solution was heated at 60° C. overnight. TLC indicated that the reaction was complete. The mixture w...
10.6084/m9.figshare.5104873.v1
null
null
Aromatic halide
c1cn[nH]c1
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1.c1ccncc1
HBr
C(C)(=O)O.CN(C)C=O
60
null
BrBr.Cn1cc(-c2ccncc2)c(-c2ccc(F)cc2)n1>C(C)(=O)O.CN(C)C=O>Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1Br
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3fcc306a9c4449289e94389f92b79ddf
Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1Br.O=Cc1ccccc1>>Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1C(O)c1ccccc1
[Mg].BrC1=C(C(=NN1C)C1=CC=C(C=C1)F)C1=CC=NC=C1.C(C1=CC=CC=C1)=O>>FC1=CC=C(C=C1)C1=NN(C(=C1C1=CC=NC=C1)C(O)C1=CC=CC=C1)C
Br[c:19]1[n:2]([CH3:1])[n:3][c:4](-[c:5]2[cH:6][cH:7][c:8]([F:9])[cH:10][cH:11]2)[c:12]1-[c:13]1[cH:14][cH:15][n:16][cH:17][cH:18]1.[CH:20](=[O:21])[c:22]1[cH:23][cH:24][cH:25][cH:26][cH:27]1>>[CH3:1][n:2]1[n:3][c:4](-[c:5]2[cH:6][cH:7][c:8]([F:9])[cH:10][cH:11]2)[c:12](-[c:13]2[cH:14][cH:15][n:16][cH:17][cH:18]2)[c:19...
Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1Br.O=Cc1ccccc1
Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1C(O)c1ccccc1
null
null
O1CCCC1
C-C Coupling
Grignard_alcohol
a9dcf423fb5579f063fb57c4002a18e05872015bf82eb9caf581a96204c0493e
1c0bd0afc1d5e370e3c8193faf738f03752295e40fa0eb99c756011e9a4be26b
c1ccc(Cc2[nH]nc(-c3ccccc3)c2-c2ccncc2)cc1
Br-[c;H0;D3;+0:1]1:[#7;a:2](-[C;D1;H3:3]):[#7;a:4]:[c:5](-[c:6]):[c:7]:1-[c:8].[O;H0;D1;+0:9]=[CH;D2;+0:10]-[c:11](:[c:12]):[c:13]>>[C;D1;H3:3]-[#7;a:2]1:[#7;a:4]:[c:5](-[c:6]):[c:7](-[c:8]):[c;H0;D3;+0:1]:1-[CH;D3;+0:10](-[OH;D1;+0:9])-[c:11](:[c:12]):[c:13]
12
[{"value": 12.0, "product": "FC1=CC=C(C=C1)C1=NN(C(=C1C1=CC=NC=C1)C(O)C1=CC=CC=C1)C", "details": "PERCENTYIELD", "is_desired": false}]
40
CELSIUS
null
null
To solid magnesium (60 mg, 5 mmol) under nitrogen was added a solution of 4-[5-bromo-3-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl]pyridine (450 mg, 1.35 mmol) (prepared in accordance with Example A-214) in tetrahydrofuran (7 mL). The mixture was heated at 40° C. for 2 hours. Benzaldehyde (1 mL) was added. The mixture wa...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Aldehyde
Secondary alcohol
c1cn[nH]c1
c1cn[nH]c1
c1cn[nH]c1.c1ccccc1.c1ccncc1.c1ccccc1
Br-
O1CCCC1
40
null
Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1Br.O=Cc1ccccc1>O1CCCC1>Cn1nc(-c2ccc(F)cc2)c(-c2ccncc2)c1C(O)c1ccccc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-1c08ee51d78245dbbfb5572cd408d2d8
CN(C)C(OC(C)(C)C)N(C)C.Cc1ccnc(Br)c1>>CN(C)/C=C/c1ccnc(Br)c1.Cc1ccnc(Br)c1
CC1=CC(=NC=C1)Br.C(C)(C)(C)OC(N(C)C)N(C)C>>CC1=CC(=NC=C1)Br.BrC1=NC=CC(=C1)/C=C/N(C)C
O([CH:4]([N:2]([CH3:1])[CH3:3])[N:17]([CH3:16])[CH3:18])[C:14]([CH3:13])([CH3:15])[CH3:20].[CH3:5][c:6]1[cH:7][cH:8][n:9][c:10]([Br:11])[cH:12]1>>[CH3:1][N:2]([CH3:3])/[CH:4]=[CH:5]/[c:6]1[cH:7][cH:8][n:9][c:10]([Br:11])[cH:12]1.[CH3:13][c:14]1[cH:15][cH:16][n:17][c:18]([Br:19])[cH:20]1
CN(C)C(OC(C)(C)C)N(C)C.Cc1ccnc(Br)c1
CN(C)/C=C/c1ccnc(Br)c1.Cc1ccnc(Br)c1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
fb4c51aec19f24da9bb69263455ca40f02e025a61b854e9b0c007a8d0f5b9341
fbe49a0e081bcdf53905cf8a3d57c67bfe6297c0544f2c3236f9be6fefa0316d
c1ccncc1.c1ccncc1
[C;D1;H3:1]-[C;H0;D4;+0:2](-[CH3;D1;+0:3])(-[CH3;D1;+0:4])-O-[CH;D3;+0:5](-[#7:6](-[C;D1;H3:7])-[C;D1;H3:8])-[N;H0;D3;+0:9](-[CH3;D1;+0:10])-[CH3;D1;+0:11].[CH3;D1;+0:12]-[c:13]1:[c:14]:[c:15]:[#7;a:16]:[c:17]:[c:18]:1>>[Br;D1;H0:19]-[c;H0;D3;+0:11]1:[cH;D2;+0:4]:[c;H0;D3;+0:2](-[C;D1;H3:1]):[cH;D2;+0:3]:[cH;D2;+0:10]:...
null
[]
null
null
null
null
4-Methyl-2-bromopyridine (1.0 g, 5.8 mmol) and t-butoxybis(dimethylamino)methane (5 ml) were heated to 150° C. for 16 hours. 4-Methyl-2-bromopyridine was prepared as set forth in B. Adger et al., J. Chem. Soc., Perkin Trans. 1, pp. 2791-2796 (1988), which is incorporated herein by reference. The contents were evaporate...
10.6084/m9.figshare.5104873.v1
null
Ether.Tertiary amine
Enamine.Aromatic halide
null
c1ccncc1
c1ccncc1.c1ccncc1
null
null
null
null
CN(C)C(OC(C)(C)C)N(C)C.Cc1ccnc(Br)c1>>CN(C)/C=C/c1ccnc(Br)c1.Cc1ccnc(Br)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-52f9731d22ea41209e8550b5e70cad66
CN(C)/C=C(\C(=O)c1cccc(Cl)c1)c1ccnc(Br)c1.NN>>Clc1cccc(-c2n[nH]cc2-c2ccnc(Br)c2)c1
BrC1=NC=CC(=C1)/C(/C(=O)C1=CC(=CC=C1)Cl)=C/N(C)C.O.NN>>BrC1=NC=CC(=C1)C=1C(=NNC1)C1=CC(=CC=C1)Cl
CN(C)/[CH:10]=[C:11](\[C:7](=O)[c:6]1[cH:5][cH:4][cH:3][c:2]([Cl:1])[cH:19]1)[c:12]1[cH:13][cH:14][n:15][c:16]([Br:17])[cH:18]1.[NH2:8][NH2:9]>>[Cl:1][c:2]1[cH:3][cH:4][cH:5][c:6](-[c:7]2[n:8][nH:9][cH:10][c:11]2-[c:12]2[cH:13][cH:14][n:15][c:16]([Br:17])[cH:18]2)[cH:19]1
CN(C)/C=C(\C(=O)c1cccc(Cl)c1)c1ccnc(Br)c1.NN
Clc1cccc(-c2n[nH]cc2-c2ccnc(Br)c2)c1
null
null
C(C)O
Aromatic Heterocycle Formation
OtherReaction
dfa2b000ac131205a53cbf7deffa11f27024f31fbf093f64d70ab7e9db936435
5904d01f33f3f511a876efed92dcef694c128bcdc48700898ac39b754505c633
c1ccc(-c2n[nH]cc2-c2ccncc2)cc1
C-N(-C)/[CH;D2;+0:1]=[C;H0;D3;+0:2](\[C;H0;D3;+0:3](=O)-[c;H0;D3;+0:4](:[c:5]:[c:6]):[c:7]:[c:8])-[c;H0;D3;+0:9]1:[c:10]:[c:11]:[#7;a:12]:[c:13](-[Br;D1;H0:14]):[c:15]:1.[NH2;D1;+0:16]-[NH2;D1;+0:17]>>[Br;D1;H0:14]-[c:13]1:[#7;a:12]:[c:11]:[c:10]:[c;H0;D3;+0:9](-[c;H0;D3;+0:2]2:[cH;D2;+0:1]:[nH;D2;+0:17]:[n;H0;D2;+0:16...
31.5
[{"value": 31.0, "product": "BrC1=NC=CC(=C1)C=1C(=NNC1)C1=CC(=CC=C1)Cl", "details": "PERCENTYIELD", "is_desired": false}, {"value": 31.5, "product": "BrC1=NC=CC(=C1)C=1C(=NNC1)C1=CC(=CC=C1)Cl", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of the product from step 2 (650 mg, 1.8 mmol) and hydrazine monohydrate (100 mg) in ethanol (10 ml) was refluxed for 24 hours. Solvent was evaporated and the residue was chromatographed on silica gel using mixtures of ethyl acetate and toluene as eluents to give 2-bromo-4-(3-(3-chlorophenyl)-1H-pyrazol-4-yl]...
10.6084/m9.figshare.5104873.v1
null
Enamine.Hydrazine.Ketone
null
null
c1cn[nH]c1
c1ccccc1.c1cn[nH]c1.c1ccncc1
HO-
C(C)O
null
null
CN(C)/C=C(\C(=O)c1cccc(Cl)c1)c1ccnc(Br)c1.NN>C(C)O>Clc1cccc(-c2n[nH]cc2-c2ccnc(Br)c2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-805e8a619eca4ce6bf9ab6f1424716a9
NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1>>Clc1cccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)c2)c1
ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(NC=C1)=NN>>ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(=NC=C1)NCC1=CC=CC=C1
N[N:17]=[c:16]1[nH:15][cH:14][cH:13][c:12](-[c:11]2[c:7](-[c:6]3[cH:5][cH:4][cH:3][c:2]([Cl:1])[cH:26]3)[n:8][nH:9][cH:10]2)[cH:25]1>>[Cl:1][c:2]1[cH:3][cH:4][cH:5][c:6](-[c:7]2[n:8][nH:9][cH:10][c:11]2-[c:12]2[cH:13][cH:14][n:15][c:16]([NH:17][CH2:18][c:19]3[cH:20][cH:21][cH:22][cH:23][cH:24]3)[cH:25]2)[cH:26]1
NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1
Clc1cccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)c2)c1
null
null
C(C1=CC=CC=C1)N
Aromatic Heterocycle Formation
OtherReaction
78ab757a26a83873db78c850941655096b12e1a71e064e5bc1dcc6122f9f5c93
fcfdaaee7721f8ca8af96a4ef99464dd31764b71786fa1482394754d563f919f
c1ccc(CNc2cc(-c3c[nH]nc3-c3ccccc3)ccn2)cc1
N-[N;H0;D2;+0:1]=[c;H0;D3;+0:2]1:[c:3]:[c:4]:[c:5]:[c:6]:[nH;D2;+0:7]:1>>[c:8]-[C:9]-[NH;D2;+0:1]-[c;H0;D3;+0:2]1:[c:3]:[c:4]:[c:5]:[c:6]:[n;H0;D2;+0:7]:1
121.9
[{"value": 61.0, "product": "ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(=NC=C1)NCC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 121.9, "product": "ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(=NC=C1)NCC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of the bromopyridine compound prepared in step 3 of Example A-219 (150 mg, 0.5 mmol) in benzylamine (5 ml) was heated at 175° C. for six hours. After cooling, excess benzylamine was removed by high vacuum distillation and ethyl acetate added to the residue. After washing the organic phase with water and dryi...
10.6084/m9.figshare.5104873.v1
null
Hydrazone
Secondary amine
c1ccncc1
c1ccncc1.c1ccccc1
c1ccccc1.c1cn[nH]c1.c1ccncc1.c1ccccc1
null
C(C1=CC=CC=C1)N
null
null
NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1>C(C1=CC=CC=C1)N>Clc1cccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)c2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b118a07e98b94ec0b7cc0223ff7ca087
NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1>>Clc1cccc(-c2n[nH]cc2-c2ccnc(NCCc3ccccc3)c2)c1
ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(NC=C1)=NN>>ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(=NC=C1)NCCC1=CC=CC=C1
N[N:17]=[c:16]1[nH:15][cH:14][cH:13][c:12](-[c:11]2[c:7](-[c:6]3[cH:5][cH:4][cH:3][c:2]([Cl:1])[cH:27]3)[n:8][nH:9][cH:10]2)[cH:26]1>>[Cl:1][c:2]1[cH:3][cH:4][cH:5][c:6](-[c:7]2[n:8][nH:9][cH:10][c:11]2-[c:12]2[cH:13][cH:14][n:15][c:16]([NH:17][CH2:18][CH2:19][c:20]3[cH:21][cH:22][cH:23][cH:24][cH:25]3)[cH:26]2)[cH:27]...
NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1
Clc1cccc(-c2n[nH]cc2-c2ccnc(NCCc3ccccc3)c2)c1
null
null
C(CC1=CC=CC=C1)N
Aromatic Heterocycle Formation
OtherReaction
78ab757a26a83873db78c850941655096b12e1a71e064e5bc1dcc6122f9f5c93
fcfdaaee7721f8ca8af96a4ef99464dd31764b71786fa1482394754d563f919f
c1ccc(CCNc2cc(-c3c[nH]nc3-c3ccccc3)ccn2)cc1
N-[N;H0;D2;+0:1]=[c;H0;D3;+0:2]1:[c:3]:[c:4]:[c:5]:[c:6]:[nH;D2;+0:7]:1>>[C:8]-[C:9]-[NH;D2;+0:1]-[c;H0;D3;+0:2]1:[c:3]:[c:4]:[c:5]:[c:6]:[n;H0;D2;+0:7]:1
163.6
[{"value": 81.0, "product": "ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(=NC=C1)NCCC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 163.6, "product": "ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(=NC=C1)NCCC1=CC=CC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of the bromopyridine compound prepared in step 3 of Example A-219 (250 mg, 0.75 mmol) in phenethylamine (5 ml) was heated at 175° C. for six hours under a nitrogen atmosphere. The excess amine was distilled off under high vacuum and the residue was dissolved in ethyl acetate and washed with water. After dryi...
10.6084/m9.figshare.5104873.v1
null
Hydrazone
Secondary amine
c1ccncc1
c1ccncc1.c1ccccc1
c1ccccc1.c1cn[nH]c1.c1ccncc1.c1ccccc1
null
C(CC1=CC=CC=C1)N
null
null
NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1>C(CC1=CC=CC=C1)N>Clc1cccc(-c2n[nH]cc2-c2ccnc(NCCc3ccccc3)c2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-ac2c04c0de4642518cbd5506b709b302
CCN.NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1>>CCNc1cc(-c2c[nH]nc2-c2cccc(Cl)c2)ccn1
ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(NC=C1)=NN.C(C)N>>ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(=NC=C1)NCC
[CH3:1][CH2:2][NH2:3].NN=[c:4]1[cH:5][c:6](-[c:7]2[cH:8][nH:9][n:10][c:11]2-[c:12]2[cH:13][cH:14][cH:15][c:16]([Cl:17])[cH:18]2)[cH:19][cH:20][nH:21]1>>[CH3:1][CH2:2][NH:3][c:4]1[cH:5][c:6](-[c:7]2[cH:8][nH:9][n:10][c:11]2-[c:12]2[cH:13][cH:14][cH:15][c:16]([Cl:17])[cH:18]2)[cH:19][cH:20][n:21]1
CCN.NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1
CCNc1cc(-c2c[nH]nc2-c2cccc(Cl)c2)ccn1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
3770d647e174bb367c3dad1a16aec780a9d143a2723b6680d9719dcab7945370
a2cc61f64635a67d464928ccd0df2bfeb2b24dd9e52bbc1660da6cc142ef8b59
c1ccc(-c2n[nH]cc2-c2ccncc2)cc1
N-N=[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[c:5]:[nH;D2;+0:6]:1.[C;D1;H3:7]-[C:8]-[NH2;D1;+0:9]>>[C;D1;H3:7]-[C:8]-[NH;D2;+0:9]-[c;H0;D3;+0:1]1:[c:2]:[c:3]:[c:4]:[c:5]:[n;H0;D2;+0:6]:1
46
[{"value": 46.0, "product": "ClC=1C=C(C=CC1)C1=NNC=C1C1=CC(=NC=C1)NCC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of the bromopyridine compound prepared in step 3 of Example A-219 (300 mg, 0.9 mmol) in ethylamine (3.5 ml) and ethanol (5 ml) as heated at 150° C. in a sealed tube for 9 hours. The solvent was removed in vacuo and the residue chromatographed on silica gel with 70 ethyl acetate/30 toluene to give 4-[3-(3-chl...
10.6084/m9.figshare.5104873.v1
null
Hydrazone.Primary amine
Secondary amine
c1ccncc1
c1ccncc1
c1ccncc1.c1cn[nH]c1.c1ccccc1
Other
C(C)O
null
null
CCN.NN=c1cc(-c2c[nH]nc2-c2cccc(Cl)c2)cc[nH]1>C(C)O>CCNc1cc(-c2c[nH]nc2-c2cccc(Cl)c2)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b34faaad8aa14c18968d85846f049561
N#Cc1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1.OO>>NC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
O.FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C#N.OO.C([O-])([O-])=O.[K+].[K+]>>FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)N
[N:1]#[C:2][c:4]1[cH:5][c:6](-[c:7]2[cH:8][nH:9][n:10][c:11]2-[c:12]2[cH:13][cH:14][c:15]([F:16])[cH:17][cH:18]2)[cH:19][cH:20][n:21]1.O[OH:3]>>[NH2:1][C:2](=[O:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][nH:9][n:10][c:11]2-[c:12]2[cH:13][cH:14][c:15]([F:16])[cH:17][cH:18]2)[cH:19][cH:20][n:21]1
N#Cc1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1.OO
NC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
null
null
CS(=O)C
Heteroatom Alkylation and Arylation
Nitrile and hydrogen peroxide to amide
b438c1a5a5f49012c6adf1e24ab44bc669089beaf4e5b0289cbfa931d3ceafda
37ed9176b981633816a0414a3f5b39ee33c11d757fe87a2cac8fe30b523bffdf
c1ccc(-c2n[nH]cc2-c2ccncc2)cc1
O-[OH;D1;+0:1].[N;H0;D1;+0:2]#[C;H0;D2;+0:3]-[c:4](:[c:5]):[#7;a:6]:[c:7]>>[NH2;D1;+0:2]-[C;H0;D3;+0:3](=[O;H0;D1;+0:1])-[c:4](:[c:5]):[#7;a:6]:[c:7]
283.4
[{"value": 67.0, "product": "FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)N", "details": "PERCENTYIELD", "is_desired": false}, {"value": 283.4, "product": "FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)N", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1
HOUR
To a solution of 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyridinecarbonitrile from step 2 (0.45 g, 0.0017 mol) in 10 mL of DMSO was added hydrogen peroxide (0.24 mL of 30% aqueous solution, 1.7 mmol) and potassium carbonate (0.04 g, 0.4 mmol) at 0° C. The mixture was stirred for 1 hour while allowing it to warm to roo...
10.6084/m9.figshare.5104873.v1
null
Nitrile.Peroxide
Primary amide
null
null
c1ccncc1.c1cn[nH]c1.c1ccccc1
Other
CS(=O)C
null
1
N#Cc1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1.OO>CS(=O)C>NC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-60cddbfe744d4b25a0c0e3447c68e8b0
COC(OC)N(C)C.NC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1>>COC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)N.COC(N(C)C)OC>>FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)OC
COC(N(C)C)[O:2][CH3:1].N[C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][nH:10][n:11][c:12]2-[c:13]2[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]2)[cH:20][cH:21][n:22]1>>[CH3:1][O:2][C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][nH:10][n:11][c:12]2-[c:13]2[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]2)[cH:20][cH:21][n:22]1
COC(OC)N(C)C.NC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
COC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
null
null
CO
Acylation
OtherReaction
595d6bd126de87caac15f4e8c9976d7f117bf8a94adb3dc2e6e2e4c519efe623
a5f18927c129d13b1e22363113e65847b548ef26b7e04f9d405e8894819737be
c1ccc(-c2n[nH]cc2-c2ccncc2)cc1
C-O-C(-[O;H0;D2;+0:1]-[C;D1;H3:2])-N(-C)-C.N-[C;H0;D3;+0:3](=[O;D1;H0:4])-[c:5](:[c:6]):[#7;a:7]:[c:8]>>[C;D1;H3:2]-[O;H0;D2;+0:1]-[C;H0;D3;+0:3](=[O;D1;H0:4])-[c:5](:[c:6]):[#7;a:7]:[c:8]
69
[{"value": 69.0, "product": "FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
To a suspension of 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyridinecarboxamide prepared as set forth in Example A-223 (2.9 g, 0.01 mol) in 50 mL of methanol was added N,N-dimethylformamide dimethyl acetal (3.67 g, 0.03 mol) dropwise. The reaction mixture was stirred at room temperature overnight and heated at reflux f...
10.6084/m9.figshare.5104873.v1
null
Ether.Ether.Primary amide.Tertiary amine
Ester
null
null
c1ccncc1.c1cn[nH]c1.c1ccccc1
HO-
CO
null
8
COC(OC)N(C)C.NC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1>CO>COC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-48bc566224a84ed6a6938877093be0f6
CN.COC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1>>CNC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)OC.CN>>FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)NC
[CH3:1][NH2:2].CO[C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][nH:10][n:11][c:12]2-[c:13]2[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]2)[cH:20][cH:21][n:22]1>>[CH3:1][NH:2][C:3](=[O:4])[c:5]1[cH:6][c:7](-[c:8]2[cH:9][nH:10][n:11][c:12]2-[c:13]2[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]2)[cH:20][cH:21][n:22]1
CN.COC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
CNC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
null
null
O
Acylation
Aminolysis of esters
04c54ce22aa9bc0cea0de3d900446bcab51cf02bebeb606fa788a47dcd0e37ff
4335147c9ad02004b7c12428d7eac0b2e7e0e2017adc471d01c387239de8017d
c1ccc(-c2n[nH]cc2-c2ccncc2)cc1
C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#7;a:5]:[c:6].[C;D1;H3:7]-[NH2;D1;+0:8]>>[C;D1;H3:7]-[NH;D2;+0:8]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[c:3](:[c:4]):[#7;a:5]:[c:6]
null
[]
120
CELSIUS
null
null
A mixture of methyl 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyridinecarboxylate prepared as set forth in Example A-224 (0.45 g, 1.5 mmol) and 20 mL of methylamine (40% aqueous solution) was heated at 120° C. in a sealed tube for 16 hours. After cooling, water was added and the aqueous phase was extracted with ethyl ac...
10.6084/m9.figshare.5104873.v1
null
Ester.Primary amine
Secondary amide
null
null
c1ccncc1.c1cn[nH]c1.c1ccccc1
HO-
O
120
null
CN.COC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1>O>CNC(=O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-921dbc232a2141aa8b536cfbd0a60f74
O=C([O-])c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1>>O=C(O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)[O-].[OH-].[Na+]>>FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)O
[O:1]=[C:2]([O-:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][nH:9][n:10][c:11]2-[c:12]2[cH:13][cH:14][c:15]([F:16])[cH:17][cH:18]2)[cH:19][cH:20][n:21]1>>[O:1]=[C:2]([OH:3])[c:4]1[cH:5][c:6](-[c:7]2[cH:8][nH:9][n:10][c:11]2-[c:12]2[cH:13][cH:14][c:15]([F:16])[cH:17][cH:18]2)[cH:19][cH:20][n:21]1
O=C([O-])c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
O=C(O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
null
null
O.C(C)O
Reduction
Carboxylate to carboxylic acid
65edb34f59b888c9ecb87d6c8e9fd76d082de6afc49403d96c457f834c73148e
222e2311064b3cb906d6bdeba44711f5dada050c096bbbcc7b35038975f228e8
c1ccc(-c2n[nH]cc2-c2ccncc2)cc1
[#7;a:1]:[c:2]-[C:3](-[O-;H0;D1:4])=[O;D1;H0:5]>>[#7;a:1]:[c:2]-[C:3](=[O;D1;H0:5])-[OH;D1;+0:4]
73
[{"value": 73.0, "product": "FC1=CC=C(C=C1)C1=NNC=C1C1=CC(=NC=C1)C(=O)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyridinecarboxylate prepared as set forth in Example A-224 (0.90 g, 0.003 mol) in 10 mL of ethanol was added a solution of sodium hydroxide (0.24 g, 0.006 mol) in 5 mL of water. The reaction mixture was heated at reflux for 10 hours. After the removal of solvent...
10.6084/m9.figshare.5104873.v1
null
null
Carboxylic acid
null
null
c1ccncc1.c1cn[nH]c1.c1ccccc1
null
O.C(C)O
null
null
O=C([O-])c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1>O.C(C)O>O=C(O)c1cc(-c2c[nH]nc2-c2ccc(F)cc2)ccn1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-557205710d604952badc543a9a9745f7
COC(OC)N(C)C.O=C(Cc1ccnc(Cl)n1)c1ccc(F)cc1>>CN(C)/C=C(/C(=O)c1ccc(F)cc1)c1ccnc(Cl)n1
ClC1=NC=CC(=N1)CC(=O)C1=CC=C(C=C1)F.COC(N(C)C)OC>>ClC1=NC=CC(=N1)/C(/C(=O)C1=CC=C(C=C1)F)=C\N(C)C
CO[CH:4](OC)[N:2]([CH3:1])[CH3:3].[CH2:5]([C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([F:12])[cH:13][cH:14]1)[c:15]1[cH:16][cH:17][n:18][c:19]([Cl:20])[n:21]1>>[CH3:1][N:2]([CH3:3])/[CH:4]=[C:5](/[C:6](=[O:7])[c:8]1[cH:9][cH:10][c:11]([F:12])[cH:13][cH:14]1)[c:15]1[cH:16][cH:17][n:18][c:19]([Cl:20])[n:21]1
COC(OC)N(C)C.O=C(Cc1ccnc(Cl)n1)c1ccc(F)cc1
CN(C)/C=C(/C(=O)c1ccc(F)cc1)c1ccnc(Cl)n1
null
null
null
C-C Coupling
OtherReaction
57f48fac7254684faf48980af66a0d538cb8dee0ab05f049059285d4840b8be4
49ae3600e90e05c7cda8811d9438748b91211f407b3eab7b1bcb51e798f4d85a
[CH]=C(C(=O)c1ccccc1)c1ccncn1
C-O-[CH;D3;+0:1](-O-C)-[#7:2](-[C;D1;H3:3])-[C;D1;H3:4].[O;D1;H0:5]=[C:6](-[c:7])-[CH2;D2;+0:8]-[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1>>[C;D1;H3:3]-[#7:2](-[C;D1;H3:4])/[CH;D2;+0:1]=[C;H0;D3;+0:8](/[C:6](=[O;D1;H0:5])-[c:7])-[c:9]1:[#7;a:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1
null
[]
null
null
8
HOUR
A mixture of the compound prepared in step 2 (4.7 g, 0.017 mol) in 100 mL of dimethylformamide dimethyl acetal was stirred at room temperature overnight. Excess dimethylformamide dimethyl acetal was removed under vacuum to give 4.5 g of crude product as a thick brown oil, which was used without further purification. Co...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ether.Ether
Enamine
null
null
c1ccccc1.c1cncnc1
HO-
null
null
8
COC(OC)N(C)C.O=C(Cc1ccnc(Cl)n1)c1ccc(F)cc1>>CN(C)/C=C(/C(=O)c1ccc(F)cc1)c1ccnc(Cl)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-444fac7d088041daa1c2a3c8dd57edce
CN(C)/C=C(/C(=O)c1ccc(F)cc1)c1ccnc(Cl)n1.NN>>Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1
ClC1=NC=CC(=N1)/C(/C(=O)C1=CC=C(C=C1)F)=C\N(C)C.O.NN>>ClC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F
CN(C)/[CH:9]=[C:10](/[C:6](=O)[c:5]1[cH:4][cH:3][c:2]([F:1])[cH:19][cH:18]1)[c:11]1[cH:12][cH:13][n:14][c:15]([Cl:16])[n:17]1.[NH2:7][NH2:8]>>[F:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][nH:8][cH:9][c:10]2-[c:11]2[cH:12][cH:13][n:14][c:15]([Cl:16])[n:17]2)[cH:18][cH:19]1
CN(C)/C=C(/C(=O)c1ccc(F)cc1)c1ccnc(Cl)n1.NN
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1
null
null
null
Aromatic Heterocycle Formation
OtherReaction
dfa2b000ac131205a53cbf7deffa11f27024f31fbf093f64d70ab7e9db936435
5904d01f33f3f511a876efed92dcef694c128bcdc48700898ac39b754505c633
c1ccc(-c2n[nH]cc2-c2ccncn2)cc1
C-N(-C)/[CH;D2;+0:1]=[C;H0;D3;+0:2](/[C;H0;D3;+0:3](=O)-[c;H0;D3;+0:4](:[c:5]:[c:6]):[c:7]:[c:8])-[c;H0;D3;+0:9]1:[#7;a:10]:[c:11](-[Cl;D1;H0:12]):[#7;a:13]:[c:14]:[c:15]:1.[NH2;D1;+0:16]-[NH2;D1;+0:17]>>[Cl;D1;H0:12]-[c:11]1:[#7;a:13]:[c:14]:[c:15]:[c;H0;D3;+0:9](-[c;H0;D3;+0:2]2:[cH;D2;+0:1]:[nH;D2;+0:17]:[n;H0;D2;+0...
48.1
[{"value": 48.1, "product": "ClC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
null
null
A solution of the compound prepared in step 3 (4.4 g) and hydrazine hydrate (0.82 g, 0.014 mol) was stirred at room temperature for 6 hours. The yellow precipitate was collected by filtration and air-dried to give 1.85 g of 2-chloro-4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]pyrimidine as a yellow solid, mp: 204-205° C.; An...
10.6084/m9.figshare.5104873.v1
null
Enamine.Hydrazine.Ketone
null
null
c1cn[nH]c1
c1ccccc1.c1cn[nH]c1.c1cncnc1
HO-
null
null
null
CN(C)/C=C(/C(=O)c1ccc(F)cc1)c1ccnc(Cl)n1.NN>>Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-507202d3eb7145aca8d59b99a4f65adf
CN.Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1>>CNc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
ClC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F.CN>>FC1=CC=C(C=C1)C1=NNC=C1C1=NC(=NC=C1)NC
[CH3:1][NH2:2].Cl[c:3]1[n:4][cH:5][cH:6][c:7](-[c:8]2[cH:9][nH:10][n:11][c:12]2-[c:13]2[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]2)[n:20]1>>[CH3:1][NH:2][c:3]1[n:4][cH:5][cH:6][c:7](-[c:8]2[cH:9][nH:10][n:11][c:12]2-[c:13]2[cH:14][cH:15][c:16]([F:17])[cH:18][cH:19]2)[n:20]1
CN.Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1
CNc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
c38b7155556ff28144ae37859ff6668b20d59da60c705d26b158542b6d8385da
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(-c2n[nH]cc2-c2ccncn2)cc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].[C;D1;H3:6]-[NH2;D1;+0:7]>>[C;D1;H3:6]-[NH;D2;+0:7]-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5]
null
[]
100
CELSIUS
null
null
A suspension of 2-chloro-4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]pyrimidine prepared in accordance with Example A-299 (0.3 g, 0.0011 mol) in 10 mL of methylamine (40% water solution) was heated in a sealed tube at 100° C. overnight. The mixture was then cooled to room temperature and the precipitate was filtered, air-dri...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1cncnc1
c1cncnc1
c1cncnc1.c1cn[nH]c1.c1ccccc1
HCl
null
100
null
CN.Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1>>CNc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-47778ad10aac4ff2a711d212a18b5a25
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1>>Fc1ccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)n2)cc1
ClC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F>>FC1=CC=C(C=C1)C1=NNC=C1C1=NC(=NC=C1)NCC1=CC=CC=C1
Cl[c:15]1[n:14][cH:13][cH:12][c:11](-[c:10]2[c:6](-[c:5]3[cH:4][cH:3][c:2]([F:1])[cH:26][cH:17]3)[n:7][nH:8][cH:9]2)[n:16]1>>[F:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][nH:8][cH:9][c:10]2-[c:11]2[cH:12][cH:13][n:14][c:15]([NH:16][CH2:17][c:18]3[cH:19][cH:20][cH:21][cH:22][cH:23]3)[n:24]2)[cH:25][cH:26]1
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1
Fc1ccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)n2)cc1
null
null
C(C1=CC=CC=C1)N
Aromatic Heterocycle Formation
OtherReaction
f414cdc2ebd114672a29511220b1d1b701c7a5d7e3abef7f1fd791da8adc5b0d
b0f572ad6b2b446ecd070d99ad48b6b5e87dc037ba48cc85596343bac1b77f42
c1ccc(CNc2nccc(-c3c[nH]nc3-c3ccccc3)n2)cc1
Cl-[c;H0;D3;+0:1]1:[#7;a:2]:[c:3]:[c:4]:[c;H0;D3;+0:5](-[c:6]2:[c:7]:[#7;a:8]:[#7;a:9]:[c:10]:2-[c;H0;D3;+0:11]2:[c:12]:[c:13]:[c:14](-[F;D1;H0:15]):[cH;D2;+0:16]:[cH;D2;+0:17]:2):[n;H0;D2;+0:18]:1>>[F;D1;H0:15]-[c:14]1:[c:13]:[c:12]:[c;H0;D3;+0:11](-[c:10]2:[#7;a:9]:[#7;a:8]:[c:7]:[c:6]:2-[c;H0;D3;+0:5]2:[#7;a:19]:[c;...
95
[{"value": 95.0, "product": "FC1=CC=C(C=C1)C1=NNC=C1C1=NC(=NC=C1)NCC1=CC=CC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
This compound was synthesize by refluxing 2-chloro-4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]pyrimidine prepared in accordance with Example A-299 in benzylamine overnight. The product, 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-N-(phenylmethyl)-2-pyrimidinamine, was obtained as a white solid in 95% yield; mp: 216-217° C.; Anal...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide
Secondary amine
c1cncnc1.c1ccccc1
c1ccccc1.c1cncnc1.c1ccccc1
c1ccccc1.c1cn[nH]c1.c1cncnc1.c1ccccc1
null
C(C1=CC=CC=C1)N
null
null
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1>C(C1=CC=CC=C1)N>Fc1ccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)n2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-3eacffbe941e42079c0771b9a848e2a1
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1.NC1CC1>>Fc1ccc(-c2n[nH]cc2-c2ccnc(NC3CC3)n2)cc1
ClC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F.C1(CC1)N>>C1(CC1)NC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F
Cl[c:15]1[n:14][cH:13][cH:12][c:11](-[c:10]2[c:6](-[c:5]3[cH:4][cH:3][c:2]([F:1])[cH:22][cH:21]3)[n:7][nH:8][cH:9]2)[n:20]1.[NH2:16][CH:17]1[CH2:18][CH2:19]1>>[F:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][nH:8][cH:9][c:10]2-[c:11]2[cH:12][cH:13][n:14][c:15]([NH:16][CH:17]3[CH2:18][CH2:19]3)[n:20]2)[cH:21][cH:22]1
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1.NC1CC1
Fc1ccc(-c2n[nH]cc2-c2ccnc(NC3CC3)n2)cc1
null
null
CO
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
c38b7155556ff28144ae37859ff6668b20d59da60c705d26b158542b6d8385da
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(-c2n[nH]cc2-c2ccnc(NC3CC3)n2)cc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].[NH2;D1;+0:6]-[C:7]1-[C:8]-[C:9]-1>>[c:5]:[#7;a:4]:[c;H0;D3;+0:1](-[NH;D2;+0:6]-[C:7]1-[C:8]-[C:9]-1):[#7;a:2]:[c:3]
26
[{"value": 26.0, "product": "C1(CC1)NC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
This compound was synthesized by stirring 2-chloro-4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]pyrimidine prepared in accordance with Example A-299 with excess cyclopropylamine in methanol at 50° C. for 12 hours. The product, N-cyclopropyl-4-(3-(4-fluorophenyl)-1H-pyrazol-4-yl)-2-pyrimidinamine, was obtained as a white solid...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1cncnc1
c1cncnc1
c1ccccc1.c1cn[nH]c1.c1cncnc1.C1CC1
HCl
CO
null
null
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1.NC1CC1>CO>Fc1ccc(-c2n[nH]cc2-c2ccnc(NC3CC3)n2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-7ad8c779d296451c9fe0a61f950921a6
COc1ccc(CN)cc1.Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1>>COc1ccc(CNc2nccc(-c3c[nH]nc3-c3ccc(F)cc3)n2)cc1
ClC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F.COC1=CC=C(CN)C=C1>>FC1=CC=C(C=C1)C1=NNC=C1C1=NC(=NC=C1)NCC1=CC=C(C=C1)OC
[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][NH2:8])[cH:27][cH:28]1.Cl[c:9]1[n:10][cH:11][cH:12][c:13](-[c:14]2[cH:15][nH:16][n:17][c:18]2-[c:19]2[cH:20][cH:21][c:22]([F:23])[cH:24][cH:25]2)[n:26]1>>[CH3:1][O:2][c:3]1[cH:4][cH:5][c:6]([CH2:7][NH:8][c:9]2[n:10][cH:11][cH:12][c:13](-[c:14]3[cH:15][nH:16][n:17][c:18]3-[c:1...
COc1ccc(CN)cc1.Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1
COc1ccc(CNc2nccc(-c3c[nH]nc3-c3ccc(F)cc3)n2)cc1
null
null
null
Heteroatom Alkylation and Arylation
N-arylation (Buchwald-Hartwig/Ullmann-Goldberg)
c38b7155556ff28144ae37859ff6668b20d59da60c705d26b158542b6d8385da
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(CNc2nccc(-c3c[nH]nc3-c3ccccc3)n2)cc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].[NH2;D1;+0:6]-[C:7]-[c:8]>>[c:3]:[#7;a:2]:[c;H0;D3;+0:1](-[NH;D2;+0:6]-[C:7]-[c:8]):[#7;a:4]:[c:5]
80
[{"value": 80.0, "product": "FC1=CC=C(C=C1)C1=NNC=C1C1=NC(=NC=C1)NCC1=CC=C(C=C1)OC", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
This compound was synthesized by refluxing 2-chloro-4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]pyrimidine prepared in accordance with Example A-299 in 4-methoxybenzylamine overnight. The product, 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-N-[(4-methoxyphenyl)methyl]-2-pyrimidinamine, was obtained as a off-white solid in 80% yie...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1cncnc1
c1cncnc1
c1ccccc1.c1cncnc1.c1cn[nH]c1.c1ccccc1
HCl
null
null
null
COc1ccc(CN)cc1.Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1>>COc1ccc(CNc2nccc(-c3c[nH]nc3-c3ccc(F)cc3)n2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8a35d8e72a834eba9ed520931875ceb5
CC(=O)OC(C)=O.Fc1ccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)n2)cc1>>CC(=O)N(Cc1ccccc1)c1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
FC1=CC=C(C=C1)C1=NNC=C1C1=NC(=NC=C1)NCC1=CC=CC=C1.C(C)(=O)OC(C)=O.C(C)N(CC)CC>>FC1=CC=C(C=C1)C1=NNC=C1C1=NC(=NC=C1)N(C(C)=O)CC1=CC=CC=C1
CC(=O)O[C:2]([CH3:1])=[O:3].[NH:4]([CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1)[c:12]1[n:13][cH:14][cH:15][c:16](-[c:17]2[cH:18][nH:19][n:20][c:21]2-[c:22]2[cH:23][cH:24][c:25]([F:26])[cH:27][cH:28]2)[n:29]1>>[CH3:1][C:2](=[O:3])[N:4]([CH2:5][c:6]1[cH:7][cH:8][cH:9][cH:10][cH:11]1)[c:12]1[n:13][cH:14][cH:15][c:16](-...
CC(=O)OC(C)=O.Fc1ccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)n2)cc1
CC(=O)N(Cc1ccccc1)c1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
null
CN(C)C=1C=CN=CC1
C1CCOC1
Acylation
Aminolysis of esters
72a6d1966b6b15ac7195d4682af251dc9ffac857f784a4242970ab5c7a529369
6593c6062585994f02076cd3c86920ae7244b86659eab65c21b5a8628c6d4bb8
c1ccc(CNc2nccc(-c3c[nH]nc3-c3ccccc3)n2)cc1
C-C(=O)-O-[C;H0;D3;+0:1](-[C;D1;H3:2])=[O;D1;H0:3].[c:4]:[#7;a:5]:[c:6](-[NH;D2;+0:7]-[C:8]-[c:9]):[#7;a:10]:[c:11]>>[C;D1;H3:2]-[C;H0;D3;+0:1](=[O;D1;H0:3])-[N;H0;D3;+0:7](-[C:8]-[c:9])-[c:6](:[#7;a:5]:[c:4]):[#7;a:10]:[c:11]
null
[]
null
null
8
HOUR
To a mixture of 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-N-(phenylmethyl)-2-pyrimidinamine prepared in accordance with Example A-303 (0.15 g, 0.00043 mol), DMAP (0.027 g, 0.00022 mol) and acetic anhydride (0.066 g, 0.00066 mol) in 10 mL of THF was added triethylamine (0.053 g, 0.00052 mol). The solution was stirred at ro...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Secondary amine
Tertiary amide
null
null
c1ccccc1.c1cncnc1.c1cn[nH]c1.c1ccccc1
HO-
CN(C)C=1C=CN=CC1.C1CCOC1
null
8
CC(=O)OC(C)=O.Fc1ccc(-c2n[nH]cc2-c2ccnc(NCc3ccccc3)n2)cc1>CN(C)C=1C=CN=CC1.C1CCOC1>CC(=O)N(Cc1ccccc1)c1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-332c3dbc1271454ab55d4fb27ca04f5b
CCOC(=O)Cl.Nc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1>>CCOC(=O)Nc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
O.FC1=CC=C(C=C1)C1=NNC=C1C1=NC(=NC=C1)N.C1=CN=C(N=C1)NS(=O)(=O)C2=CC=C(C=C2)N.ClC(=O)OCC>>C(C)OC(NC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F)=O
Cl[C:4]([O:3][CH2:2][CH3:1])=[O:5].[NH2:6][c:7]1[n:8][cH:9][cH:10][c:11](-[c:12]2[cH:13][nH:14][n:15][c:16]2-[c:17]2[cH:18][cH:19][c:20]([F:21])[cH:22][cH:23]2)[n:24]1>>[CH3:1][CH2:2][O:3][C:4](=[O:5])[NH:6][c:7]1[n:8][cH:9][cH:10][c:11](-[c:12]2[cH:13][nH:14][n:15][c:16]2-[c:17]2[cH:18][cH:19][c:20]([F:21])[cH:22][cH:...
CCOC(=O)Cl.Nc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
CCOC(=O)Nc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
null
null
N1=CC=CC=C1
Protection
Acylation of Nitrogen Nucleophiles by Acyl/Thioacyl/Carbamoyl Halides and Analogs_OS
038720aa61a7efa0f2a9ee6f2e0adf63a9ffdc2be4697c11a6215baef34f97b2
205f353513ce9506ab61831799da8fb73ec2ef5cfa927664496d3ce72c438860
c1ccc(-c2n[nH]cc2-c2ccncn2)cc1
Cl-[C;H0;D3;+0:1](=[O;D1;H0:2])-[#8:3]-[C:4].[NH2;D1;+0:5]-[c:6](:[#7;a:7]:[c:8]):[#7;a:9]:[c:10]>>[C:4]-[#8:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[NH;D2;+0:5]-[c:6](:[#7;a:7]:[c:8]):[#7;a:9]:[c:10]
null
[]
null
null
6
HOUR
To a suspension of 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyrimidinamine prepared in accordance with Example A-306 (0.26 g, 0.001 mol) in 5 mL of pyridine was added ethyl chloroformate dropwise. After the addition, the clear solution was stirred at room temperature for 6 hours. Water was added and the aqueous phase w...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Ether.Primary amine
Carbamic ester
null
null
c1cncnc1.c1cn[nH]c1.c1ccccc1
HCl
N1=CC=CC=C1
null
6
CCOC(=O)Cl.Nc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1>N1=CC=CC=C1>CCOC(=O)Nc1nccc(-c2c[nH]nc2-c2ccc(F)cc2)n1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-f063ce1a31b14145937e680188c797d5
CC[C@H](C)[C@H](NC(=O)[C@H](CO)NC(=O)[C@H](C)NC(=O)[C@H](C)N)C(=O)N[C@@H](CCCCN)C(=O)N[C@H](C(=O)N[C@@H](C)C(=O)N[C@H](C(=O)N[C@@H](CO)C(=O)N[C@@H](C)C(=O)N[C@@H](CC(=O)O)C(=O)N[C@@H](CCCN=C(N)N)C(=O)O)C(C)C)C(C)C.COC(=O)c1cccc(C)c1.Cc1ccncn1.O=C(Cc1ccncc1)c1ccc(F)cc1>>Cc1cccc(-c2n[nH]cc2-c2ccncn2)c1
CC=1C=C(C(=O)OC)C=CC1.CC[C@H](C)[C@@H](C(=O)N[C@@H](CCCCN)C(=O)N[C@@H](C(C)C)C(=O)N[C@@H](C)C(=O)N[C@@H](C(C)C)C(=O)N[C@@H](CO)C(=O)N[C@@H](C)C(=O)N[C@@H](CC(=O)O)C(=O)N[C@@H](CCCN=C(N)N)C(=O)O)NC(=O)[C@H](CO)NC(=O)[C@H](C)NC(=O)[C@H](C)N.FC1=CC=C(C(=O)CC2=CC=NC=C2)C=C1.CC1=NC=NC=C1>>CC=1C=C(C=CC1)C1=NNC=C1C1=NC=NC=C1
CC[C@H](C)[C@H](NC(=O)[C@H](CO)NC(=O)[C@H](C)NC(=O)[C@H](C)N)C(=O)N[C@@H](CCCCN)C(=O)[NH:8][C@H](C(=O)N[C@@H](C)C(=O)N[C@H](C(=O)N[C@@H](CO)C(=O)N[C@@H](C)C(=O)N[C@@H](CC(=O)O)C(=O)N[C@@H](CCCN=C(N)N)C(=O)O)C(C)C)C(C)C.CO[C:7](=O)[c:6]1[cH:5][cH:4][cH:3][c:2]([CH3:1])[cH:18]1.[CH3:11][c:12]1[cH:13][cH:14][n:15][cH:16][...
CC[C@H](C)[C@H](NC(=O)[C@H](CO)NC(=O)[C@H](C)NC(=O)[C@H](C)N)C(=O)N[C@@H](CCCCN)C(=O)N[C@H](C(=O)N[C@@H](C)C(=O)N[C@H](C(=O)N[C@@H](CO)C(=O)N[C@@H](C)C(=O)N[C@@H](CC(=O)O)C(=O)N[C@@H](CCCN=C(N)N)C(=O)O)C(C)C)C(C)C.COC(=O)c1cccc(C)c1.Cc1ccncn1.O=C(Cc1ccncc1)c1ccc(F)cc1
Cc1cccc(-c2n[nH]cc2-c2ccncn2)c1
null
null
null
Miscellaneous
OtherReaction
5d185fa330956694446a5ce13c104e9c2fe8d95e6592b182417951877b53016a
8fd360cfe649c09aa9c4ca06ea883331a0800bec68f3cb05a1b6221ccce33e79
c1ccc(-c2n[nH]cc2-c2ccncn2)cc1
C-C-[C@H](-C)-[C@H](-N-C(=O)-[C@H](-C-O)-N-C(=O)-[C@H](-C)-N-C(=O)-[C@H](-C)-N)-C(=O)-N-[C@@H](-C-C-C-C-N)-C(=O)-[NH;D2;+0:1]-[C@H](-C(-C)-C)-C(=O)-N-[C@@H](-C)-C(=O)-N-[C@H](-C(-C)-C)-C(=O)-N-[C@@H](-C-O)-C(=O)-N-[C@@H](-C)-C(=O)-N-[C@@H](-C-C(-O)=O)-C(=O)-N-[C@@H](-C-C-C-N=C(-N)-N)-C(-O)=O.C-O-[C;H0;D3;+0:2](=O)-[c;H...
null
[]
null
null
null
null
This compound was prepared by the same procedure as described for Example A-208 except that 1-methyl-3-(4′-pyrimidinylacetyl) benzene (prepared as set forth in Step 1 of Example A-19 from 4-methyl-pyrimidine and methyl 3-methylbenzoate) was used in place of 4-fluorobenzoyl-4-pyridinyl methane. Conditions: See reaction....
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Carboxylic acid.Carboxylic acid.Ketone.Ester.Secondary amide.Secondary amide.Secondary amide.Secondary amide.Secondary amide.Secondary amide.Secondary amide.Secondary amide.Secondary amide.Secondary amide.Secondary amide.Primary alcohol.Primary alcohol.Primary amine.Primary amine.Primary amine.Primary a...
null
c1ccncc1.c1ccccc1
c1cn[nH]c1
c1ccccc1.c1cn[nH]c1.c1cncnc1
HF
null
null
null
CC[C@H](C)[C@H](NC(=O)[C@H](CO)NC(=O)[C@H](C)NC(=O)[C@H](C)N)C(=O)N[C@@H](CCCCN)C(=O)N[C@H](C(=O)N[C@@H](C)C(=O)N[C@H](C(=O)N[C@@H](CO)C(=O)N[C@@H](C)C(=O)N[C@@H](CC(=O)O)C(=O)N[C@@H](CCCN=C(N)N)C(=O)O)C(C)C)C(C)C.COC(=O)c1cccc(C)c1.Cc1ccncn1.O=C(Cc1ccncc1)c1ccc(F)cc1>>Cc1cccc(-c2n[nH]cc2-c2ccncn2)c1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-29ac42e35fb54511a6e1cdaf8ed77d68
Cc1[nH]nc(-c2ccc(F)cc2)c1-c1ccncc1.[O]=[Mn](=[O])(=[O])[O-]>>O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
O.FC1=CC=C(C=C1)C1=NNC(=C1C1=CC=NC=C1)C.[Mn](=O)(=O)(=O)[O-].[K+].[Mn](=O)(=O)(=O)[O-].[K+]>>O.FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)O)C1=CC=NC=C1
[CH3:3][c:5]1[nH:6][n:7][c:8](-[c:9]2[cH:10][cH:11][c:12]([F:13])[cH:14][cH:15]2)[c:16]1-[c:17]1[cH:18][cH:19][n:20][cH:21][cH:22]1.[O]=[Mn](=[O])(=[O:2])[O-:4]>>[O:2]=[C:3]([OH:4])[c:5]1[n:6][nH:7][c:8](-[c:9]2[cH:10][cH:11][c:12]([F:13])[cH:14][cH:15]2)[c:16]1-[c:17]1[cH:18][cH:19][n:20][cH:21][cH:22]1
Cc1[nH]nc(-c2ccc(F)cc2)c1-c1ccncc1.[O]=[Mn](=[O])(=[O])[O-]
O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
null
null
C(C)(C)(C)O
Acylation
OtherReaction
7769a4cd09a67e270ac2d1d32df6b7a59b468ff590f9c59723b72ba3c8deb342
903e48d04e4504a4fe6977f5e5582144adff237d0488a4542a1907161cf0134c
c1ccc(-c2[nH]ncc2-c2ccncc2)cc1
[CH3;D1;+0:1]-[c:2]1:[c:3]:[c:4](-[c:5]):[n;H0;D2;+0:6]:[nH;D2;+0:7]:1.[O-;H0;D1:8]-[Mn](=[O;H0;D1;+0:9])(=[O])=[O]>>[O;H0;D1;+0:9]=[C;H0;D3;+0:1](-[OH;D1;+0:8])-[c:2]1:[c:3]:[c:4](-[c:5]):[nH;D2;+0:6]:[n;H0;D2;+0:7]:1
40.6
[{"value": 40.6, "product": "O.FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)O)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
8
HOUR
A mixture of 4-[3-(4-fluorophenyl)-5-methyl-1H-pyrazol-4-yl)pyridine (5.8 g, 24.0909 mmol; prepared as set forth in Example A-4) and potassium permanganate (7.6916 g, 48.1818 mmol) in water (7.5 mL) and tert-butanol (10 mL) was heated to reflux at 95 to 100° C. for 6 hours (or until all the potassium permanganate was c...
10.6084/m9.figshare.5104873.v1
null
null
Carboxylic acid
null
null
c1cn[nH]c1.c1ccccc1.c1ccncc1
HO-
C(C)(C)(C)O
null
8
Cc1[nH]nc(-c2ccc(F)cc2)c1-c1ccncc1.[O]=[Mn](=[O])(=[O])[O-]>C(C)(C)(C)O>O=C(O)c1n[nH]c(-c2ccc(F)cc2)c1-c1ccncc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-48d632ca4e0f40deb2677fcf9e2654d8
CC(C)(C)OC(=O)N1CCN(C(=O)c2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1>>CN1CCN(Cc2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1
FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)N1CCN(CC1)C(=O)OC(C)(C)C)C1=CC=NC=C1.[OH-].[K+].CO.C(C)(=O)OCC.[NH4+].[OH-]>>FC1=CC=C(C=C1)C1=C(C(=NN1)CN1CCN(CC1)C)C1=CC=NC=C1
CC(C)(C)O[C:1](=O)[N:2]1[CH2:3][CH2:4][N:5]([C:6](=O)[c:7]2[n:8][nH:9][c:10](-[c:11]3[cH:12][cH:13][c:14]([F:15])[cH:16][cH:17]3)[c:18]2-[c:19]2[cH:20][cH:21][n:22][cH:23][cH:24]2)[CH2:25][CH2:26]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([CH2:6][c:7]2[n:8][nH:9][c:10](-[c:11]3[cH:12][cH:13][c:14]([F:15])[cH:16][cH:17]3)[c:18...
CC(C)(C)OC(=O)N1CCN(C(=O)c2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1
CN1CCN(Cc2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1
null
null
O1CCCC1.O.[H-].[H-].[H-].[H-].[Li+].[Al+3].C(C)(=O)OCC
Reduction
OtherReaction
d1e38ff76373f2f85a70c476a5d7ea2d461bd8feff67e57b568219071b445e34
e3e848d08b64607479a3af6f757302d1c3f585ca2558bd4bfb2ce28c641ade14
c1ccc(-c2[nH]nc(CN3CCNCC3)c2-c2ccncc2)cc1
C-C(-C)(-C)-O-[C;H0;D3;+0:1](=O)-[#7:2]1-[C:3]-[C:4]-[#7:5](-[C;H0;D3;+0:6](=O)-[c:7]2:[#7;a:8]:[#7;a:9]:[c:10]:[c:11]:2)-[C:12]-[C:13]-1>>[CH3;D1;+0:1]-[#7:2]1-[C:3]-[C:4]-[#7:5](-[CH2;D2;+0:6]-[c:7]2:[#7;a:8]:[#7;a:9]:[c:10]:[c:11]:2)-[C:12]-[C:13]-1
50.1
[{"value": 50.1, "product": "FC1=CC=C(C=C1)C1=C(C(=NN1)CN1CCN(CC1)C)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}, {"value": 43.0, "product": "FC1=CC=C(C=C1)C1=C(C(=NN1)CN1CCN(CC1)C)C1=CC=NC=C1", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
1.5
HOUR
To a suspension of 1,1-dimethylethyl 4-[[5-(4-fluorophenyl)-4-(4-pyridinyl)-1H-pyrazol-3-yl]carbonyl]-1-piperazinecarboxylate (0.451 g, 1.0 mL) in dry tetrahydrofuran (8 mL), 1.0N LiAlH4 in tetrahydrofuran (2.5 mL, 2.5 mmol) was added dropwise at such a rate as to maintain reflux over 15 minutes. Upon the addition, the...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Tertiary amide.Boc
null
null
null
C1C[NH]CC[NH]1.c1cn[nH]c1.c1ccccc1.c1ccncc1
HO-
O1CCCC1.O.[H-].[H-].[H-].[H-].[Li+].[Al+3].C(C)(=O)OCC
null
1.5
CC(C)(C)OC(=O)N1CCN(C(=O)c2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1>O1CCCC1.O.[H-].[H-].[H-].[H-].[Li+].[Al+3].C(C)(=O)OCC>CN1CCN(Cc2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-78ee5e4781a84148947e6b81bd1b4bd5
CCOC(=O)CC1CCN(C(=O)OC(C)(C)C)CC1.Cc1ccncc1>>CC(C)(C)OC(=O)N1CCC(CC(=O)Cc2ccncc2)CC1
[Cl-].[Ce+3].[Cl-].[Cl-].C(C)(C)[N-]C(C)C.C(CCC)[Li].CCCCCC.N1=CC=C(C=C1)C.C(C)(C)[N-]C(C)C.[Li+].C(C)(C)[N-]C(C)C.[Li+].CC(C)(OC(=O)N1CCC(CC1)CC(=O)OCC)C>>O=C(CC1CCN(CC1)C(=O)OC(C)(C)C)CC1=CC=NC=C1
CCO[C:13]([CH2:12][CH:11]1[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:23][CH2:22]1)=[O:14].[CH3:15][c:16]1[cH:17][cH:18][n:19][cH:20][cH:21]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][C:13](=[O:14])[CH2:15][c:16]2[cH:17][cH:18][n:19][cH:20][cH:...
CCOC(=O)CC1CCN(C(=O)OC(C)(C)C)CC1.Cc1ccncc1
CC(C)(C)OC(=O)N1CCC(CC(=O)Cc2ccncc2)CC1
null
null
C(C)(=O)OCC.CCCCCC.O1CCCC1
C-C Coupling
OtherReaction
8ce89878f5db9b98fa4633d16adf2407dbf79d96925d930c608f1ce0756e674e
f80cbbd7f2bfc042e62829b7de30498cf0880b808f2adad888ffdfe089982722
O=C(Cc1ccncc1)CC1CCNCC1
C-C-O-[C;H0;D3;+0:1](=[O;D1;H0:2])-[C:3]-[C:4].[CH3;D1;+0:5]-[c:6]1:[c:7]:[c:8]:[#7;a:9]:[c:10]:[c:11]:1>>[C:4]-[C:3]-[C;H0;D3;+0:1](=[O;D1;H0:2])-[CH2;D2;+0:5]-[c:6]1:[c:7]:[c:8]:[#7;a:9]:[c:10]:[c:11]:1
25
[{"value": 25.0, "product": "O=C(CC1CCN(CC1)C(=O)OC(C)(C)C)CC1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
-78
CELSIUS
1.5
HOUR
To a solution of diisopropylamide (6.15 mL, 43.91 mmol) in dry tetrahydrofuran (40 mL) at 0° C. was added 2.5 M butyl lithium solution in hexane (16.22 mL, 40.53 mmol) dropwise over 10 minutes. After the addition, the lithium diisopropylamide solution was stirred at 0° C. for 20 minutes, then cooled to −78° C. 4-Picoli...
10.6084/m9.figshare.5104873.v1
null
Ester
Ketone
null
null
C1CC[NH]CC1.c1ccncc1
HO-
C(C)(=O)OCC.CCCCCC.O1CCCC1
-78
1.5
CCOC(=O)CC1CCN(C(=O)OC(C)(C)C)CC1.Cc1ccncc1>C(C)(=O)OCC.CCCCCC.O1CCCC1>CC(C)(C)OC(=O)N1CCC(CC(=O)Cc2ccncc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-2004ca65deec472ebfed350e5c6220a7
CC(C)(C)OC(=O)N1CCC(CC(=O)Cc2ccncc2)CC1.O=Cc1ccc(F)cc1>>CC(C)(C)OC(=O)N1CCC(CC(=O)C(=Cc2ccc(F)cc2)c2ccncc2)CC1
FC1=CC=C(C=O)C=C1.N1=CC=C(C=C1)CC(C)=O.FC=1C=C(C=O)C=CC1OC.O=C(CC1CCN(CC1)C(=O)OC(C)(C)C)CC1=CC=NC=C1>>FC1=CC=C(C=C1)C=C(C(CC1CCN(CC1)C(=O)OC(C)(C)C)=O)C1=CC=NC=C1
[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][C:13](=[O:14])[CH2:15][c:24]2[cH:25][cH:26][n:27][cH:28][cH:29]2)[CH2:30][CH2:31]1.O=[CH:16][c:17]1[cH:18][cH:19][c:20]([F:21])[cH:22][cH:23]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][C:13...
CC(C)(C)OC(=O)N1CCC(CC(=O)Cc2ccncc2)CC1.O=Cc1ccc(F)cc1
CC(C)(C)OC(=O)N1CCC(CC(=O)C(=Cc2ccc(F)cc2)c2ccncc2)CC1
null
null
null
C-C Coupling
Aldol condensation
df1bdbab1a06af9561d74fe6bc94ee8bda1d14faad9db1ada3a214bd64a24cf8
c93e93ada40f7f922a54fe24d38f540ecf5ff25d55d497f79f5f400f75d0c7ae
O=C(CC1CCNCC1)C(=Cc1ccccc1)c1ccncc1
O=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4].[C:5]-[C:6](=[O;D1;H0:7])-[CH2;D2;+0:8]-[c:9]1:[c:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1>>[C:5]-[C:6](=[O;D1;H0:7])-[C;H0;D3;+0:8](=[CH;D2;+0:1]-[c:2](:[c:3]):[c:4])-[c:9]1:[c:10]:[c:11]:[#7;a:12]:[c:13]:[c:14]:1
null
[]
null
null
null
null
1,1-Dimethylethyl 4-[4-(4-fluorophenyl)-2-oxo-3-(4-pyridinyl)-3-butenyl]-1-piperidinecarboxylate was prepared by the same method as described for step 1 of Example A-1 by replacing 4-pyridylacetone and 3-fluoro-p-anisaldehyde with the ketone of step 2 of the present Example and 4-fluorobenzaldehyde, respectively. Condi...
10.6084/m9.figshare.5104873.v1
null
Aldehyde.Ketone
Ketone
null
null
C1CC[NH]CC1.c1ccccc1.c1ccncc1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(CC(=O)Cc2ccncc2)CC1.O=Cc1ccc(F)cc1>>CC(C)(C)OC(=O)N1CCC(CC(=O)C(=Cc2ccc(F)cc2)c2ccncc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-e777a6ab67484a6788036952d7e3878b
CC(=O)C(=Cc1ccccc1)c1ccncc1.CC(C)(C)OC(=O)N1CCC(CC(=O)C(=Cc2ccc(F)cc2)c2ccncc2)CC1>>CC(C)(C)OC(=O)N1CCC(CC(=O)C2(c3ccncc3)OC2c2ccc(F)cc2)CC1
C1(=CC=CC=C1)C=C(C(C)=O)C1=CC=NC=C1.FC1=CC=C(C=C1)C=C(C(CC1CCN(CC1)C(=O)OC(C)(C)C)=O)C1=CC=NC=C1>>FC1=CC=C(C=C1)C1C(O1)(C1=CC=NC=C1)C(CC1CCN(CC1)C(=O)OC(C)(C)C)=O
CC(C(=Cc1ccccc1)c1ccncc1)=[O:22].[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][CH:11]([CH2:12][C:13](=[O:14])[C:15]([c:16]2[cH:17][cH:18][n:19][cH:20][cH:21]2)=[CH:23][c:24]2[cH:25][cH:26][c:27]([F:28])[cH:29][cH:30]2)[CH2:31][CH2:32]1>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:...
CC(=O)C(=Cc1ccccc1)c1ccncc1.CC(C)(C)OC(=O)N1CCC(CC(=O)C(=Cc2ccc(F)cc2)c2ccncc2)CC1
CC(C)(C)OC(=O)N1CCC(CC(=O)C2(c3ccncc3)OC2c2ccc(F)cc2)CC1
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
24e5a88ce69d7c2c82159f3a967c4e67572dd01e387f05153ff2a48694ec7bd7
ab6b65f5e9f2eb3ba4b4737f10d104b1ae24afb168129247d60e743fa5ac8b83
O=C(CC1CCNCC1)C1(c2ccncc2)OC1c1ccccc1
C-C(=[O;H0;D1;+0:1])-C(=C-c1:c:c:c:c:c:1)-c1:c:c:n:c:c:1.[C:2]-[C:3](=[O;D1;H0:4])-[C;H0;D3;+0:5](=[CH;D2;+0:6]-[c:7](:[c:8]):[c:9])-[c:10]1:[c:11]:[c:12]:[#7;a:13]:[c:14]:[c:15]:1>>[C:2]-[C:3](=[O;D1;H0:4])-[C;H0;D4;+0:5]1(-[c:10]2:[c:11]:[c:12]:[#7;a:13]:[c:14]:[c:15]:2)-[O;H0;D2;+0:1]-[CH;D3;+0:6]-1-[c:7](:[c:8]):[c...
null
[]
null
null
null
null
1,1-Dimethylethyl 4-(2-[3-(4-fluorophenyl)-2-(4-pyridinyl)oxiranyl]-2-oxoethyl]-1-piperidinecarboxylate was prepared by the same method as described for step 3 of Example A-2 by replacing 4-phenyl-3-(4-pyridyl)-3-butene-2-one with the α,β unsaturated ketone of step 3 of the present Example. Conditions: See reaction.not...
10.6084/m9.figshare.5104873.v1
null
Ketone.Ketone
Ketone.Ether
c1ccccc1.c1ccncc1
C1CO1
C1CC[NH]CC1.c1ccncc1.C1CO1.c1ccccc1
Other
null
null
null
CC(=O)C(=Cc1ccccc1)c1ccncc1.CC(C)(C)OC(=O)N1CCC(CC(=O)C(=Cc2ccc(F)cc2)c2ccncc2)CC1>>CC(C)(C)OC(=O)N1CCC(CC(=O)C2(c3ccncc3)OC2c2ccc(F)cc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-d11da7ec693843858f9cb323ee94d22b
CC(C)(C)OC(=O)N1CCC(CC(=O)C2(c3ccncc3)OC2c2ccc(F)cc2)CC1.NN>>CC(C)(C)OC(=O)N1CCC(CC2=NNC(c3ccc(F)cc3)C2(O)c2ccncc2)CC1
FC1=CC=C(C=C1)C1C(O1)(C1=CC=NC=C1)C(CC1CCN(CC1)C(=O)OC(C)(C)C)=O.NN>>FC1=CC=C(C=C1)C1C(C(=NN1)CC1CCN(CC1)C(=O)OC(C)(C)C)(C1=CC=NC=C1)O
O=[C:13]([CH2:12][CH:11]1[CH2:10][CH2:9][N:8]([C:6]([O:5][C:2]([CH3:1])([CH3:3])[CH3:4])=[O:7])[CH2:33][CH2:32]1)[C:24]1([c:26]2[cH:27][cH:28][n:29][cH:30][cH:31]2)[CH:16]([c:17]2[cH:18][cH:19][c:20]([F:21])[cH:22][cH:23]2)[O:25]1.[NH2:14][NH2:15]>>[CH3:1][C:2]([CH3:3])([CH3:4])[O:5][C:6](=[O:7])[N:8]1[CH2:9][CH2:10][C...
CC(C)(C)OC(=O)N1CCC(CC(=O)C2(c3ccncc3)OC2c2ccc(F)cc2)CC1.NN
CC(C)(C)OC(=O)N1CCC(CC2=NNC(c3ccc(F)cc3)C2(O)c2ccncc2)CC1
null
null
C(C)O
Heteroatom Alkylation and Arylation
OtherReaction
413aebc198e33af37de46cc9dc029a0a6e192f19d16a03f65d960d12511c5bf0
58e6d8eaf186f1d0e9a62408070dce07b35e7010855b0bf338cff7a37f228f81
c1ccc(C2NN=C(CC3CCNCC3)C2c2ccncc2)cc1
O=[C;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]1(-[c:5])-[O;H0;D2;+0:6]-[CH;D3;+0:7]-1-[c:8](:[c:9]):[c:10].[NH2;D1;+0:11]-[NH2;D1;+0:12]>>[C:3]-[C:2]-[C;H0;D3;+0:1]1=[N;H0;D2;+0:11]-[NH;D2;+0:12]-[CH;D3;+0:7](-[c:8](:[c:9]):[c:10])-[C:4]-1(-[OH;D1;+0:6])-[c:5]
53.9
[{"value": 53.9, "product": "FC1=CC=C(C=C1)C1C(C(=NN1)CC1CCN(CC1)C(=O)OC(C)(C)C)(C1=CC=NC=C1)O", "details": "PERCENTYIELD", "is_desired": false}]
null
null
null
null
To a solution of 1,1-dimethylethyl 4-[2-[3-(4-fluorophenyl)-2-(4-pyridinyl)oxiranyl]-2-oxoethyl]-1-piperidinecarboxylate prepared in step 4 of this Example (3.45 g, 7.8409 mmol) in ethanol (15 mL), anhydrous hydrazine (0.50 mL, 15.6818 mmol) was added. The reaction was heated to reflux overnight. The reaction solution ...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Ether
Hydrazone.Tertiary alcohol
C1CO1
C1=NNCC1
C1CC[NH]CC1.C1=NNCC1.c1ccccc1.c1ccncc1
HO-
C(C)O
null
null
CC(C)(C)OC(=O)N1CCC(CC(=O)C2(c3ccncc3)OC2c2ccc(F)cc2)CC1.NN>C(C)O>CC(C)(C)OC(=O)N1CCC(CC2=NNC(c3ccc(F)cc3)C2(O)c2ccncc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-16d796de8c3d43a5b96bf661f394c01e
CC(C)(C)OC(=O)N1CCC(Cc2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1>>Fc1ccc(-c2n[nH]c(CC3CCNCC3)c2-c2ccncc2)cc1
O.FC1=CC=C(C=C1)C1=C(C(=NN1)C(=O)N1CCNCC1)C1=CC=NC=C1.FC1=CC=C(C=C1)C1=C(C(=NN1)CC1CCN(CC1)C(=O)OC(C)(C)C)C1=CC=NC=C1>>FC1=CC=C(C=C1)C1=NNC(=C1C1=CC=NC=C1)CC1CCNCC1
CC(C)(C)OC(=O)[N:14]1[CH2:13][CH2:12][CH:11]([CH2:10][c:9]2[n:8][nH:7][c:6](-[c:5]3[cH:4][cH:3][c:2]([F:1])[cH:25][cH:24]3)[c:17]2-[c:18]2[cH:19][cH:20][n:21][cH:22][cH:23]2)[CH2:16][CH2:15]1>>[F:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][nH:8][c:9]([CH2:10][CH:11]3[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]3)[c:17]2-[c:18]2[c...
CC(C)(C)OC(=O)N1CCC(Cc2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1
Fc1ccc(-c2n[nH]c(CC3CCNCC3)c2-c2ccncc2)cc1
null
null
null
Reduction
OtherReaction
bf3cd5dc3e17e694d8665c89f5d7e08e8763b18436a633eb66e9bf530b8b0316
a94b29c7264c852156fc1cdd4a0951a4fc26c06d0edc9e50c743825dbf79e3fd
c1ccc(-c2n[nH]c(CC3CCNCC3)c2-c2ccncc2)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1](-[C:2]-[C:3])-[C:4]-[C:5].[C:6]-[c:7]1:[c:8]:[c:9](-[c:10]):[nH;D2;+0:11]:[n;H0;D2;+0:12]:1>>[C:3]-[C:2]-[NH;D2;+0:1]-[C:4]-[C:5].[C:6]-[c:7]1:[c:8]:[c:9](-[c:10]):[n;H0;D2;+0:11]:[nH;D2;+0:12]:1
null
[]
null
null
null
null
4-[3-(4-Fluorophenyl)-5-(4-piperidinylmethyl)-1H-pyrazol-4-yl]pyridine was prepared using the same method as described for Example A-314, step 1 by replacing 1-[[5-(4-fluorophenyl)-4-(4-pyridinyl)-1H-pyrazol-3-yl]carbonyl]piperazine, monohydrate with the pyrazole of step 5 of the present Example. Anal. Calc'd for C20H2...
10.6084/m9.figshare.5104873.v1
null
Carbamic ester.Ether.Boc
Secondary amine
C1CC[NH]CC1
C1CCNCC1
c1ccccc1.c1cn[nH]c1.C1CCNCC1.c1ccncc1
HO-
null
null
null
CC(C)(C)OC(=O)N1CCC(Cc2n[nH]c(-c3ccc(F)cc3)c2-c2ccncc2)CC1>>Fc1ccc(-c2n[nH]c(CC3CCNCC3)c2-c2ccncc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c29682e0b23047cf9c54eab8703177eb
CC(=O)Cl.CC(C)(C)OC(=O)N1CCN(c2[nH]nc(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1.CO>>C#CCn1nc(N2CCNCC2)c(-c2ccncc2)c1-c1ccc(Cl)cc1.Cl.Cl.O
Cl.C(C)(=O)Cl.CO.CO.ClC1=CC=C(C=C1)C1=NNC(=C1C1=CC=NC=C1)N1CCN(CC1)C(=O)OC(C)(C)C>>O.Cl.Cl.Cl.ClC1=CC=C(C=C1)C1=C(C(=NN1CC#C)N1CCNCC1)C1=CC=NC=C1
O=[C:2]([CH3:3])[Cl:29].CC(C)(C)OC(=O)[N:10]1[CH2:9][CH2:8][N:7]([c:6]2[nH:5][n:4][c:20](-[c:21]3[cH:22][cH:23][c:24]([Cl:25])[cH:26][cH:27]3)[c:13]2-[c:14]2[cH:15][cH:16][n:17][cH:18][cH:19]2)[CH2:12][CH2:11]1.[CH3:1][OH:31]>>[CH:1]#[C:2][CH2:3][n:4]1[n:5][c:6]([N:7]2[CH2:8][CH2:9][NH:10][CH2:11][CH2:12]2)[c:13](-[c:1...
CC(=O)Cl.CC(C)(C)OC(=O)N1CCN(c2[nH]nc(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1.CO
C#CCn1nc(N2CCNCC2)c(-c2ccncc2)c1-c1ccc(Cl)cc1.Cl.Cl.O
null
null
null
Heteroatom Alkylation and Arylation
OtherReaction
f509b0242b4ca73794d7a7155a837586bbc4dd1506dd49122ab9f9c4a8dd4350
2b0692bf029cf8e18cf2ae87cb1e8cb3a80b7a382d953614367c22133886aba7
c1ccc(-c2[nH]nc(N3CCNCC3)c2-c2ccncc2)cc1
C-C(-C)(-C)-O-C(=O)-[N;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4](-[c:5]2:[c:6]:[c:7](-[c:8]):[n;H0;D2;+0:9]:[nH;D2;+0:10]:2)-[C:11]-[C:12]-1.O=[C;H0;D3;+0:13](-[CH3;D1;+0:14])-[Cl;H0;D1;+0:15].[CH3;D1;+0:16]-[OH;D1;+0:17]>>[CH;D1;+0:16]#[C;H0;D2;+0:13]-[CH2;D2;+0:14]-[n;H0;D3;+0:9]1:[n;H0;D2;+0:10]:[c:5](-[#7:4]2-[C:3]-[C:2]-[NH...
90
[{"value": 90.0, "product": "O.Cl.Cl.Cl.ClC1=CC=C(C=C1)C1=C(C(=NN1CC#C)N1CCNCC1)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
5
CELSIUS
1
HOUR
A solution of HCl in methanol (5 mL) was generated by addition of acetyl chloride (200 mg) to methanol while cooling (5° C.). 3-(4-Chlorophenyl)-4-(4-pyridyl)-5-(4-N-tert.-butoxycarbonylpiperazinyl)pyrazole (100 mg, 0.2 mmol) prepared above was added and the reaction stirred in the cold for one hour. The reaction mixtu...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Carbamic ester.Ether.Methanol.Boc
Secondary amine.Alkyne
C1C[NH]CC[NH]1.c1cn[nH]c1
c1cn[nH]c1.C1C[NH]CCN1
c1cn[nH]c1.C1C[NH]CCN1.c1ccncc1.c1ccccc1
HO-
null
5
1
CC(=O)Cl.CC(C)(C)OC(=O)N1CCN(c2[nH]nc(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1.CO>>C#CCn1nc(N2CCNCC2)c(-c2ccncc2)c1-c1ccc(Cl)cc1.Cl.Cl.O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8f732a621ba7431f8cd0b56120fcc158
COC(=O)Cl.COC(=O)Cl.Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1>>COC(=O)N1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1.O
ClC(=O)OC.ClC1=CC=C(C=C1)C1=NNC(=C1C1=CC=NC=C1)N1CCNCC1.ClC(=O)OC>>O.ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCN(CC1)C(=O)OC)C1=CC=NC=C1
Cl[C:3]([O:2][CH3:1])=[O:4].COC(Cl)=[O:29].[NH:5]1[CH2:6][CH2:7][N:8]([c:9]2[nH:10][n:11][c:12](-[c:13]3[cH:14][cH:15][c:16]([Cl:17])[cH:18][cH:19]3)[c:20]2-[c:21]2[cH:22][cH:23][n:24][cH:25][cH:26]2)[CH2:27][CH2:28]1>>[CH3:1][O:2][C:3](=[O:4])[N:5]1[CH2:6][CH2:7][N:8]([c:9]2[n:10][nH:11][c:12](-[c:13]3[cH:14][cH:15][c...
COC(=O)Cl.COC(=O)Cl.Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1
COC(=O)N1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1.O
null
CN(C1=CC=NC=C1)C
N1=CC=CC=C1
Protection
OtherReaction
0e02fc91170b49b5aa2dca8c80b08a118529932c2c18cd69f9b50afc29bf35d6
fed6af1de63673a8c49fb23c3aff5dc52a5e8e165cca4fe8707334eafa4bd550
c1ccc(-c2[nH]nc(N3CCNCC3)c2-c2ccncc2)cc1
C-O-C(-Cl)=[O;H0;D1;+0:1].Cl-[C;H0;D3;+0:2](=[O;D1;H0:3])-[#8:4]-[C;D1;H3:5].[c:6]-[c:7]1:[c:8]:[c:9](-[#7:10]2-[C:11]-[C:12]-[NH;D2;+0:13]-[C:14]-[C:15]-2):[nH;D2;+0:16]:[n;H0;D2;+0:17]:1>>[C;D1;H3:5]-[#8:4]-[C;H0;D3;+0:2](=[O;D1;H0:3])-[N;H0;D3;+0:13]1-[C:12]-[C:11]-[#7:10](-[c:9]2:[c:8]:[c:7](-[c:6]):[nH;D2;+0:17]:[...
48
[{"value": 48.0, "product": "O.ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCN(CC1)C(=O)OC)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
3
HOUR
Methyl chloroformate (55 mg) was added to a solution of 3-(4-chlorophenyl)-4-(4-pyridyl)-5-(4-piperazinyl)pyrazole (200 mg, 0.54 mmol; prepared as set forth in Example A-169) and 4-dimethylaminopyridine (5 mg) in pyridine (10 mL). The mixture was stirred at room temperature for 3 hours. Additional methyl chloroformate ...
10.6084/m9.figshare.5104873.v1
null
Acyl halide.Acyl halide.Ether.Ether.Secondary amine
Carbamic ester.Ether
C1CNCC[NH]1
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1cn[nH]c1.c1ccccc1.c1ccncc1
HCl
CN(C1=CC=NC=C1)C.N1=CC=CC=C1
null
3
COC(=O)Cl.COC(=O)Cl.Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1>CN(C1=CC=NC=C1)C.N1=CC=CC=C1>COC(=O)N1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1.O
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-79afce2fa3924dc5b9705bb990752660
Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1.O=C1CCC(=O)O1>>O.O.O=C(O)CCC(=O)N1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1
ClC1=CC=C(C=C1)C1=NNC(=C1C1=CC=NC=C1)N1CCNCC1.C1(CCC(=O)O1)=O>>O.O.ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCN(CC1)C(CCC(=O)O)=O)C1=CC=NC=C1
[NH:10]1[CH2:11][CH2:12][N:13]([c:14]2[nH:15][n:16][c:17](-[c:18]3[cH:19][cH:20][c:21]([Cl:22])[cH:23][cH:24]3)[c:25]2-[c:26]2[cH:27][cH:28][n:29][cH:30][cH:31]2)[CH2:32][CH2:33]1.[O:1]=[C:8]1[O:5][C:4](=[O:3])[CH2:6][CH2:7]1>>[OH2:1].[OH2:2].[O:3]=[C:4]([OH:5])[CH2:6][CH2:7][C:8](=[O:9])[N:10]1[CH2:11][CH2:12][N:13]([...
Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1.O=C1CCC(=O)O1
O.O.O=C(O)CCC(=O)N1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1
null
CN(C1=CC=NC=C1)C
null
Functional Group Addition
OtherReaction
02167a30770a77e8035d02274783b892ce713006cddb323eb2cb80946d0186fb
2b0361106072ffa92111156a29af982a2a07689a390bf1c6a6a152f5698f2dc0
c1ccc(-c2[nH]nc(N3CCNCC3)c2-c2ccncc2)cc1
[O;D1;H0:1]=[C:2]1-[C:3]-[C:4]-[C;H0;D3;+0:5](=[O;H0;D1;+0:6])-[O;H0;D2;+0:7]-1.[c:8]-[c:9]1:[c:10]:[c:11](-[#7:12]2-[C:13]-[C:14]-[NH;D2;+0:15]-[C:16]-[C:17]-2):[nH;D2;+0:18]:[n;H0;D2;+0:19]:1>>[O;D1;H0:1]=[C:2](-[OH;D1;+0:7])-[C:3]-[C:4]-[C;H0;D3;+0:5](=[O;D1;H0:20])-[N;H0;D3;+0:15]1-[C:14]-[C:13]-[#7:12](-[c:11]2:[c...
58
[{"value": 58.0, "product": "O.O.ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCN(CC1)C(CCC(=O)O)=O)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
A solution of 3-(4-chlorophenyl)-4-(4-pyridyl)-5-(4-piperzinyl)pyrazole (200 mg; 0.54 mmol; prepared as set forth in Example A-169), succinic anhydride (60 mg, 0.55 mmol) and 4-dimethylaminopyridine (5 mg) was stirred at room temperature for 24 hours. The solvent was removed in vacuo and the residue treated with methan...
10.6084/m9.figshare.5104873.v1
null
Anhydride.Secondary amine
Carboxylic acid.Tertiary amide
C1CNCC[NH]1.C1CCOC1
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1cn[nH]c1.c1ccccc1.c1ccncc1
Other
CN(C1=CC=NC=C1)C
null
24
Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1.O=C1CCC(=O)O1>CN(C1=CC=NC=C1)C>O.O.O=C(O)CCC(=O)N1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-b9af1afd69274b8d86e5c594287bb052
CCOC1(O[Si](C)(C)C)CC1.Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1>>Clc1ccc(-c2[nH]nc(N3CCN(C4CC4)CC3)c2-c2ccncc2)cc1
C(C)OC1(CC1)O[Si](C)(C)C.ClC1=CC=C(C=C1)C1=NNC(=C1C1=CC=NC=C1)N1CCNCC1.C(#N)[BH3-].[Na+].C(C)(=O)O>>ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCN(CC1)C1CC1)C1=CC=NC=C1
CCO[C:14]1(O[Si](C)(C)C)[CH2:15][CH2:16]1.[Cl:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][nH:8][c:9]([N:10]3[CH2:11][CH2:12][NH:13][CH2:17][CH2:18]3)[c:19]2-[c:20]2[cH:21][cH:22][n:23][cH:24][cH:25]2)[cH:26][cH:27]1>>[Cl:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[nH:7][n:8][c:9]([N:10]3[CH2:11][CH2:12][N:13]([CH:14]4[CH2:15][CH2:16]...
CCOC1(O[Si](C)(C)C)CC1.Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1
Clc1ccc(-c2[nH]nc(N3CCN(C4CC4)CC3)c2-c2ccncc2)cc1
null
null
CO
Heteroatom Alkylation and Arylation
OtherReaction
607f9b7d2366723fd12e941369c42f5b4c0d36ce239278f2bebe31ef811fa60c
d68204a4cfa34cff6cd0e9ec3beba0b05875e761733cc428bd8f8c7f1d92fb07
c1ccc(-c2[nH]nc(N3CCN(C4CC4)CC3)c2-c2ccncc2)cc1
C-C-O-[C;H0;D4;+0:1]1(-O-[Si](-C)(-C)-C)-[C:2]-[C:3]-1.[c:4]-[c:5]1:[c:6]:[c:7](-[#7:8]2-[C:9]-[C:10]-[NH;D2;+0:11]-[C:12]-[C:13]-2):[nH;D2;+0:14]:[n;H0;D2;+0:15]:1>>[c:4]-[c:5]1:[c:6]:[c:7](-[#7:8]2-[C:9]-[C:10]-[N;H0;D3;+0:11](-[CH;D3;+0:1]3-[C:2]-[C:3]-3)-[C:12]-[C:13]-2):[n;H0;D2;+0:14]:[nH;D2;+0:15]:1
63
[{"value": 63.0, "product": "ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCN(CC1)C1CC1)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
null
null
5
MINUTE
To a solution of 3-(4-chlorophenyl)-4-(4-pyridyl)-5-(4-piperazinyl)pyrazole (1.95-g; 5.8 mmoles; prepared as set forth in Example A-169) and acetic acid (3.6 g, 60 mmol) containing SA molecular sieves (6 g) was added [(1-ethoxycyclopropyl)oxy]trimethylsilane (6 g, 35 mmol). After stirring for 5 minutes, sodium cyanobor...
10.6084/m9.figshare.5104873.v1
null
Ether.Secondary amine.Silyl protective group
Tertiary amine
C1CC1.C1C[NH]CCN1
C1C[NH]CC[NH]1.C1CC1
c1ccccc1.c1cn[nH]c1.C1C[NH]CC[NH]1.C1CC1.c1ccncc1
HO-
CO
null
0.083333
CCOC1(O[Si](C)(C)C)CC1.Clc1ccc(-c2n[nH]c(N3CCNCC3)c2-c2ccncc2)cc1>CO>Clc1ccc(-c2[nH]nc(N3CCN(C4CC4)CC3)c2-c2ccncc2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-8a51e9fbfd424ea284f812afdea561e0
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1.Nc1ccccc1F>>Fc1ccc(-c2n[nH]cc2-c2ccnc(Nc3ccccc3F)n2)cc1
ClC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F.FC1=C(N)C=CC=C1>>FC1=C(C=CC=C1)NC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F
Cl[c:15]1[n:14][cH:13][cH:12][c:11](-[c:10]2[c:6](-[c:5]3[cH:4][cH:3][c:2]([F:1])[cH:26][cH:25]3)[n:7][nH:8][cH:9]2)[n:24]1.[NH2:16][c:17]1[cH:18][cH:19][cH:20][cH:21][c:22]1[F:23]>>[F:1][c:2]1[cH:3][cH:4][c:5](-[c:6]2[n:7][nH:8][cH:9][c:10]2-[c:11]2[cH:12][cH:13][n:14][c:15]([NH:16][c:17]3[cH:18][cH:19][cH:20][cH:21][...
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1.Nc1ccccc1F
Fc1ccc(-c2n[nH]cc2-c2ccnc(Nc3ccccc3F)n2)cc1
null
CO
null
Heteroatom Alkylation and Arylation
Goldberg coupling aryl amine-aryl chloride
c38b7155556ff28144ae37859ff6668b20d59da60c705d26b158542b6d8385da
71a04ae650defc5edd86a92f43c304e981a05f07ff76248da8d4155f3905a29d
c1ccc(Nc2nccc(-c3c[nH]nc3-c3ccccc3)n2)cc1
Cl-[c;H0;D3;+0:1](:[#7;a:2]:[c:3]):[#7;a:4]:[c:5].[NH2;D1;+0:6]-[c:7](:[c:8]):[c:9]>>[c:5]:[#7;a:4]:[c;H0;D3;+0:1](-[NH;D2;+0:6]-[c:7](:[c:8]):[c:9]):[#7;a:2]:[c:3]
77
[{"value": 77.0, "product": "FC1=C(C=CC=C1)NC1=NC=CC(=N1)C=1C(=NNC1)C1=CC=C(C=C1)F", "details": "PERCENTYIELD", "is_desired": false}]
180
CELSIUS
null
null
A mixture of 2-chloro-4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]pyrimidine (0.37 g; 0.0013 mol; prepared as set forth in Example A-299), 7 mL of 2-fluoroaniline and 2 drops of methanol was heated at 180° C. in a sealed tube for 16 hours. Excess amine was removed by vacuum distillation and the residue was treated with ethyl...
10.6084/m9.figshare.5104873.v1
null
Aromatic halide.Primary amine
Secondary amine
c1cncnc1
c1cncnc1
c1ccccc1.c1cn[nH]c1.c1cncnc1.c1ccccc1
HCl
CO
180
null
Fc1ccc(-c2n[nH]cc2-c2ccnc(Cl)n2)cc1.Nc1ccccc1F>CO>Fc1ccc(-c2n[nH]cc2-c2ccnc(Nc3ccccc3F)n2)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-6ee0bdc742a745a892e2c81122a50cd0
C=O.Clc1ccc(-c2[nH]nc(N3CCNCC3)c2-c2ccncc2)cc1>>CN1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1
ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCNCC1)C1=CC=NC=C1.C=O>>ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCN(CC1)C)C1=CC=NC=C1
O=[CH2:1].[NH:2]1[CH2:3][CH2:4][N:5]([c:6]2[n:7][nH:8][c:9](-[c:10]3[cH:11][cH:12][c:13]([Cl:14])[cH:15][cH:16]3)[c:17]2-[c:18]2[cH:19][cH:20][n:21][cH:22][cH:23]2)[CH2:24][CH2:25]1>>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([c:6]2[n:7][nH:8][c:9](-[c:10]3[cH:11][cH:12][c:13]([Cl:14])[cH:15][cH:16]3)[c:17]2-[c:18]2[cH:19][cH:20...
C=O.Clc1ccc(-c2[nH]nc(N3CCNCC3)c2-c2ccncc2)cc1
CN1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1
null
null
C(=O)O
Heteroatom Alkylation and Arylation
Eschweiler-Clarke Secondary Amine Methylation
bebbbc2e5c9880d648b53dd51b2cf84a8e9c9861f8ae46f927ebe311ad1ddfb0
e1fdef8fde1c506d7c9deb8fd5e6f322eceea2abce3167abcf412a1fa4fd5443
c1ccc(-c2[nH]nc(N3CCNCC3)c2-c2ccncc2)cc1
O=[CH2;D1;+0:1].[#7:2]1-[C:3]-[C:4]-[NH;D2;+0:5]-[C:6]-[C:7]-1>>[CH3;D1;+0:1]-[N;H0;D3;+0:5]1-[C:4]-[C:3]-[#7:2]-[C:7]-[C:6]-1
68
[{"value": 68.0, "product": "ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CCN(CC1)C)C1=CC=NC=C1", "details": "PERCENTYIELD", "is_desired": false}]
60
CELSIUS
16
HOUR
The compound of Example A-170 was also synthesized in the following manner. 1-[5-(4-Chlorophenyl)-4-(4-pyridinyl)-1H-pyrazol-3-yl]piperazine (12.2 g, 36 mmol, prepared as set forth in Example A-169), 88% formic acid (20 ml), and formaldehyde (37% formalin solution; 44 g, 540 mmol) were combined and stirred at 60° C. fo...
10.6084/m9.figshare.5104873.v1
null
Formaldehyde.Secondary amine
Tertiary amine
C1CNCC[NH]1
C1C[NH]CC[NH]1
C1C[NH]CC[NH]1.c1cn[nH]c1.c1ccccc1.c1ccncc1
Other
C(=O)O
60
16
C=O.Clc1ccc(-c2[nH]nc(N3CCNCC3)c2-c2ccncc2)cc1>C(=O)O>CN1CCN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-5e5de61c27764bc6a4d1626afe7d0a8c
O=C(Cc1ccncc1)c1ccc(Cl)cc1.S=C=S>>O=C(C(=C1SCS1)c1ccncc1)c1ccc(Cl)cc1
N1=CC=C(C=C1)CC(=O)C1=CC=C(C=C1)Cl.C([O-])([O-])=O.[K+].[K+].BrCBr.C(=S)=S.C([O-])([O-])=O.[K+].[K+].C(=S)=S>>ClC1=CC=C(C=C1)C(C(C1=CC=NC=C1)=C1SCS1)=O
[O:1]=[C:2]([CH2:3][c:8]1[cH:9][cH:10][n:11][cH:12][cH:13]1)[c:14]1[cH:15][cH:16][c:17]([Cl:18])[cH:19][cH:20]1.[C:4](=[S:5])=[S:7]>>[O:1]=[C:2]([C:3](=[C:4]1[S:5][CH2:6][S:7]1)[c:8]1[cH:9][cH:10][n:11][cH:12][cH:13]1)[c:14]1[cH:15][cH:16][c:17]([Cl:18])[cH:19][cH:20]1
O=C(Cc1ccncc1)c1ccc(Cl)cc1.S=C=S
O=C(C(=C1SCS1)c1ccncc1)c1ccc(Cl)cc1
null
null
CC(=O)C
Heteroatom Alkylation and Arylation
OtherReaction
45739c82b492cab85da91dc7e10d4ad2aca0010f979d0ecc36adfc3be01ea86d
f2df0f382e7f6df1891c311da091c26cb669c7e7671ba8f75a8e799bf7582e3d
O=C(C(=C1SCS1)c1ccncc1)c1ccccc1
[O;D1;H0:1]=[C:2](-[c:3])-[CH2;D2;+0:4]-[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1.[S;H0;D1;+0:11]=[C;H0;D2;+0:12]=[S;H0;D1;+0:13]>>[O;D1;H0:1]=[C:2](-[c:3])-[C;H0;D3;+0:4](=[C;H0;D3;+0:12]1-[S;H0;D2;+0:11]-[C:14]-[S;H0;D2;+0:13]-1)-[c:5]1:[c:6]:[c:7]:[#7;a:8]:[c:9]:[c:10]:1
81.7
[{"value": 81.7, "product": "ClC1=CC=C(C=C1)C(C(C1=CC=NC=C1)=C1SCS1)=O", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
24
HOUR
To a solution of 2-(4-pyridyl)-1-(4-chlorophenyl)ethanone (70.0 g, 0.3 mol) prepared in a similar manner as the compound of Step 1 of Example A-19, dibromomethane (200 mL) and carbon disulfide (25.9 g, 0.34 mol) in acetone (800 mL) was added potassium carbonate (83.0 g, 0.6 mol). The reaction mixture was stirred at roo...
10.6084/m9.figshare.5104873.v1
null
Ketone
Ketone.Monosulfide.Monosulfide
null
C1SCS1
C1SCS1.c1ccncc1.c1ccccc1
Other
CC(=O)C
null
24
O=C(Cc1ccncc1)c1ccc(Cl)cc1.S=C=S>CC(=O)C>O=C(C(=C1SCS1)c1ccncc1)c1ccc(Cl)cc1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-94b9789562d44bf8a7bef0413f87460b
CC1CNCC(C)N1.NN.O=C(C(=C1SCS1)c1ccncc1)c1ccc(Cl)cc1>>CC1CN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC(C)N1
NN.ClC1=CC=C(C=C1)C(C(C1=CC=NC=C1)=C1SCS1)=O.CC1NC(CNC1)C>>ClC1=CC=C(C=C1)C1=C(C(=NN1)N1CC(NC(C1)C)C)C1=CC=NC=C1
[CH3:1][CH:2]1[CH2:3][NH:4][CH2:23][CH:24]([CH3:25])[NH:26]1.[NH2:6][NH2:7].O=[C:8]([c:9]1[cH:10][cH:11][c:12]([Cl:13])[cH:14][cH:15]1)[C:16](=[C:5]1SCS1)[c:17]1[cH:18][cH:19][n:20][cH:21][cH:22]1>>[CH3:1][CH:2]1[CH2:3][N:4]([c:5]2[n:6][nH:7][c:8](-[c:9]3[cH:10][cH:11][c:12]([Cl:13])[cH:14][cH:15]3)[c:16]2-[c:17]2[cH:1...
CC1CNCC(C)N1.NN.O=C(C(=C1SCS1)c1ccncc1)c1ccc(Cl)cc1
CC1CN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC(C)N1
null
null
O1CCCC1.C1(=CC=CC=C1)C
Aromatic Heterocycle Formation
OtherReaction
4ba032ef00e1aab4abb44832e59f1d5d02c4d73b36f1a2c5cf3b1813dc5309f7
1e5f9b38d7db4fe595144f898e5235f6b6271ba8ecf3ac3e92120040e09a299c
c1ccc(-c2[nH]nc(N3CCNCC3)c2-c2ccncc2)cc1
O=[C;H0;D3;+0:1](-[C;H0;D3;+0:2](=[C;H0;D3;+0:3]1-S-C-S-1)-[c;H0;D3;+0:4]1:[c:5]:[c:6]:[#7;a:7]:[c:8]:[c:9]:1)-[c;H0;D3;+0:10](:[c:11]:[c:12]):[c:13]:[c:14].[#7:15]1-[C:16]-[C:17]-[NH;D2;+0:18]-[C:19]-[C:20]-1.[NH2;D1;+0:21]-[NH2;D1;+0:22]>>[c:12]:[c:11]:[c;H0;D3;+0:10](-[c;H0;D3;+0:1]1:[nH;D2;+0:22]:[n;H0;D2;+0:21]:[c...
null
[]
null
null
1
HOUR
A mixture of 1-(4-chlorophenyl)-2-(1,3-dithietan-2-ylidene)-2-(4-pyridinyl)ethanone (3.2 g, 0.01 mol; prepared as set forth in step 1 of Example A-341) and 2,6-dimethylpiperazine (3.43 g, 0.03 mol) in 35 mL of toluene was heated at reflux for 12 hours. Toluene and excess 2,6-dimethylpiperazine were then removed under v...
10.6084/m9.figshare.5104873.v1
null
Hydrazine.Ketone.Secondary amine.Monosulfide.Monosulfide
Tertiary amine
C1CNCCN1.C1SCS1
C1CNCC[NH]1.c1cn[nH]c1
C1CNCC[NH]1.c1cn[nH]c1.c1ccccc1.c1ccncc1
Other
O1CCCC1.C1(=CC=CC=C1)C
null
1
CC1CNCC(C)N1.NN.O=C(C(=C1SCS1)c1ccncc1)c1ccc(Cl)cc1>O1CCCC1.C1(=CC=CC=C1)C>CC1CN(c2n[nH]c(-c3ccc(Cl)cc3)c2-c2ccncc2)CC(C)N1
ord_dataset-c3a75813d0b24864aa4f7cd526efd6aa
ord-c3c882500a8d45a88c6af2dd611204ff
CN.CN1CCC(=O)CC1>>CNC1CCN(C)CC1
CN1CCC(CC1)=O.O1CCCC1.CN>>CN1CCC(CC1)NC
[CH3:1][NH2:2].O=[C:3]1[CH2:4][CH2:5][N:6]([CH3:7])[CH2:8][CH2:9]1>>[CH3:1][NH:2][CH:3]1[CH2:4][CH2:5][N:6]([CH3:7])[CH2:8][CH2:9]1
CN.CN1CCC(=O)CC1
CNC1CCN(C)CC1
null
[Pd]
CO
Heteroatom Alkylation and Arylation
Reductive amination with ketone
42e9e55fb09951ae64da272b20a0fe6708e6155493933c6a5b57bd203fbe3626
07faf85ffe990e88a1de7fd04a339bf226f78d8bfae9712ea59eebd76bb54b9f
C1CCNCC1
O=[C;H0;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1.[C;D1;H3:7]-[NH2;D1;+0:8]>>[C;D1;H3:7]-[NH;D2;+0:8]-[CH;D3;+0:1]1-[C:2]-[C:3]-[#7:4]-[C:5]-[C:6]-1
87
[{"value": 87.0, "product": "CN1CCC(CC1)NC", "details": "PERCENTYIELD", "is_desired": false}, {"value": 86.7, "product": "CN1CCC(CC1)NC", "details": "CALCULATEDPERCENTYIELD", "is_desired": false}]
null
null
2
HOUR
A mixture of 1-methyl-4-piperidone (20 g, 0.18 mol) in methanol:tetrahydrofuran (100 mL, 1:1) and methyl amine (2 M in tetrahydrofuran, 3 mole excess) was placed in a Parr shaker with 5% Pd/C and hydrogenated for two hours at 60 psi and 70° C. The catalyst was filtered and the filtrate concentrated on the rotary evapor...
10.6084/m9.figshare.5104873.v1
null
Ketone.Primary amine
Secondary amine
C1CC[NH]CC1
C1CC[NH]CC1
C1CC[NH]CC1
Other
[Pd].CO
null
2
CN.CN1CCC(=O)CC1>[Pd].CO>CNC1CCN(C)CC1