(3S)-氨基-1,3,4,5-四氢-2H-1-苯氮杂卓-2-酮

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Prepared from 3(S)-amino-2,3,4,5-tetrahydro-1H-1-benzazepin-2-on (Example 1, Step B) and 3-benzyloxycarbonylamino-3-methylbutanoic acid (Example 1, Step E) by the procedure described in Example 1, Step F. FAB-MS: calculated for C23H27N3O4 409; found 410 (M+H,100%). [a]D =-160° (C=1,CHCl3).

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: (4S,7S,10aS)-Methyl 4-((2R,5R)-2,5-dibenzyl-6-oxo-6-((S)-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-3-ylamino)hexanamido)-5-oxooctahydro-2H-pyrido[2,1-b][1,3]thiazepine-7-carboxylate was synthesized as described in General Procedure H using Intermediate 23 (5.0 mg, 0.0088 mmol) and (S)-3-amino-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one (1.6 mg, 0.0088 mmol) to give a white solid (5.1 mg, 80% yield). Anal. Calcd. for C41H48N4O6S m/z 724.9. found: 725.3 (M+H)+; 1H NMR (400 MHz, CDCl3) δ ppm 7.24-6.90 (m, 14H), 6.28-6.20 (m, 1H), 5.29-5.20 (m, 1H), 5.04-4.97 (m, 2H), 4.93-4.84 (m, 2H), 4.30-4.20 (m, 1H), 3.60-3.53 (m, 3H), 3.20-3.04 (m, 1H), 2.82-2.50 (m, 8H), 2.37-2.19 (m, 4H), 1.96-1.88 (m, 2H), 1.85-1.68 (m, 2H), 1.67-1.31 (m, 6H), 1.27-1.14 (m, 1H).

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: (4S,7S,10aS)-Methyl 4-((2R,5R)-2,5-dibenzyl-6-oxo-6-((S)-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-3-ylamino)hexanamido)-5-oxooctahydro-2H-pyrido[2,1-b][1,3]thiazepine-7-carboxylate was synthesized as described in General Procedure H using Intermediate 23 (5.0 mg, 0.0088 mmol) and (S)-3-amino-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one (1.6 mg, 0.0088 mmol) to give a white solid (5.1 mg, 80% yield). Anal. Calcd. for C41H48N4O6S m/z 724.9. found: 725.3 (M+H)+; 1H NMR (400 MHz, CDCl3) δ ppm 7.24-6.90 (m, 14H), 6.28-6.20 (m, 1H), 5.29-5.20 (m, 1H), 5.04-4.97 (m, 2H), 4.93-4.84 (m, 2H), 4.30-4.20 (m, 1H), 3.60-3.53 (m, 3H), 3.20-3.04 (m, 1H), 2.82-2.50 (m, 8H), 2.37-2.19 (m, 4H), 1.96-1.88 (m, 2H), 1.85-1.68 (m, 2H), 1.67-1.31 (m, 6H), 1.27-1.14 (m, 1H).

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Prepared from 3(S)-amino-2,3,4,5-tetrahydro-1H-1-benzazepin-2-one (Example 1, Step B) and 3-benzyloxycarbonylamino-3-methylbutanoic acid (Example 1, Step E) by the procedure described in Example 1, Step F. FAB-MS: calculated for C23H27N3O4 409; found 410 (M+H,100%). [a]D =- 160° (c=1,CHCl3).

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Prepared from 3(S)-amino-2,3,4,5-tetrahydro-1H-1-benzazepin-2-on (Example 1, Step B) and 3-benzyloxycarbonylamino-3-methylbutanoic acid (Example 1, Step E) by the procedure described in Example 1, Step F. FAB-MS: calculated for C23H27N3O4 409; found 410 (M+H,100%). [a]D =-160° (C=1,CHCl3).

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: (4S,7S,10aS)-Methyl 4-((2R,5R)-2,5-dibenzyl-6-oxo-6-((S)-2-oxo-2,3,4,5-tetrahydro-1H-benzo[b]azepin-3-ylamino)hexanamido)-5-oxooctahydro-2H-pyrido[2,1-b][1,3]thiazepine-7-carboxylate was synthesized as described in General Procedure H using Intermediate 23 (5.0 mg, 0.0088 mmol) and (S)-3-amino-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one (1.6 mg, 0.0088 mmol) to give a white solid (5.1 mg, 80% yield). Anal. Calcd. for C41H48N4O6S m/z 724.9. found: 725.3 (M+H)+; 1H NMR (400 MHz, CDCl3) δ ppm 7.24-6.90 (m, 14H), 6.28-6.20 (m, 1H), 5.29-5.20 (m, 1H), 5.04-4.97 (m, 2H), 4.93-4.84 (m, 2H), 4.30-4.20 (m, 1H), 3.60-3.53 (m, 3H), 3.20-3.04 (m, 1H), 2.82-2.50 (m, 8H), 2.37-2.19 (m, 4H), 1.96-1.88 (m, 2H), 1.85-1.68 (m, 2H), 1.67-1.31 (m, 6H), 1.27-1.14 (m, 1H).