Acetic Acid → HCID 89851602、化合物
反応式
Cl.[NH2:2][C:3](=[O:32])[CH:4]([OH:31])[CH:5]([NH:13][C:14](=[O:30])[C:15]1[CH:20]=[CH:19][CH:18]=[N:17][C:16]=1[N:21]1[CH:29]=[C:28]2[C:23]([CH2:24][NH:25][CH2:26][CH2:27]2)=[N:22]1)[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.CO.[C:35](O)(=O)[CH3:36]>>[NH2:2][C:3](=[O:32])[CH:4]([OH:31])[CH:5]([NH:13][C:14](=[O:30])[C:15]1[CH:20]=[CH:19][CH:18]=[N:17][C:16]=1[N:21]1[CH:29]=[C:28]2[C:23]([CH2:24][N:25]([CH2:35][CH3:36])[CH2:26][CH2:27]2)=[N:22]1)[CH2:6][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1参加物
4
実験手順
To a solution of N-(4-amino-3-hydroxy-4-oxo-1-phenylbutan-2-yl)-2-(4,5,6,7-tetrahydro-2H-pyrazolo[3,4-c]pyridin-2-yl)nicotinamide hydrochloride (210 mg, 0.460 mmol) in methanol (15 ml) first acetaldehyde (150 μL, 2.66 mmol) and after 30 minutes NaCN(BH4)4 (40 mg, 0.637 mmol) and glacial acetic acid (20 μL, 0.349 mmol) were added and stirred over night. The mixture was concentrated, 20 mL of water, 10 mL NaHCO3-solution and 20 mL of dichloromethane added, the organic layer separated, washed 2× with water, dried with MgSO4, filtered and concentrated to give 85 mg of an amorphous solid; ESI-MS [M+H]+: 449.2.