Hydrochloric Acid → 5-{[(1R,2S)-2-aminocyclohexyl]amino}-3-[(4,6-dimethylpyridin-2-yl)amino]pyridine-2-carboxamide hydrochloric acid salt
反応式
[C:1]([C:4]1[N:9]=[CH:8][C:7]([NH:10][C@@H:11]2[CH2:16][CH2:15][CH2:14][CH2:13][C@@H:12]2[NH:17]C(=O)OC(C)(C)C)=[CH:6][C:5]=1[NH:25][C:26]1[CH:31]=[C:30]([CH3:32])[CH:29]=[C:28]([CH3:33])[N:27]=1)(=[O:3])[NH2:2].[ClH:34]>O1CCOCC1>[ClH:34].[NH2:17][C@H:12]1[CH2:13][CH2:14][CH2:15][CH2:16][C@H:11]1[NH:10][C:7]1[CH:6]=[C:5]([NH:25][C:26]2[CH:31]=[C:30]([CH3:32])[CH:29]=[C:28]([CH3:33])[N:27]=2)[C:4]([C:1]([NH2:2])=[O:3])=[N:9][CH:8]=1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
tert-Butyl [(1S,2R)-2-({6-carbamoyl-5-[(4,6-dimethylpyridin-2-yl)amino]pyridin-3-yl]amino)cyclohexyl}carbamate (22.5 g, 49.5 mmol) was diluted with dioxane (140 mL). To this solution was added hydrochloric acid (4.0 M in dioxane, 62 mL, 250 mmol). After 30 minutes, the reaction mixture was diluted with hexanes (400 mL) and filtered. The collected solids were dried in a nitrogen bag. The solids were diluted with dioxane (140 mL) followed by hydrochloric acid (4.0 M in dioxane, 62 mL, 250 mmol). After 1 hour, the reaction mixture was diluted with hexanes (400 mL), filtered, and washed with hexanes (2×150 mL). The isolated solids were dried under reduced pressure, and then suspended in dichloromethane (300 mL). After stirring for 3 hours, the mixture was filtered and dried in a nitrogen bag to afford 5-{[(1R,2S)-2-aminocyclohexyl]amino}-3-[(4,6-dimethylpyridin-2-yl)amino]pyridine-2-carboxamide hydrochloric acid salt.