反应详情

To a stirred solution of 2-(trimethylacetylamino)-6-[(4-t-butoxycarbonylamino-1-piperidinyl)methyl]pyridine formic acid salt (0.74 g, 3.0 mmol) in methanol (6 mL) was added 6 N HCl (2 mL) at room temperature. The resulting mixture was heated to reflux for 10 h. Then, the reaction was cooled to room temperature and concentrated under rotary evaporator. After azeotropic removal of water with 1-propanol twice (20 mL each), the resulting solid was treated with methanol (5 mL). After being stirred for 1 h in methanol, ethanol (12 mL) was added slowly and stirred for additional 1 h. After filtration, drying of the resulting crystalline solid gave the desired title compound (491 mg, 80% yield, 98 A % purity).

1. temperatureThe resulting mixture was heated
2. temperatureto reflux for 10 h
3. concentrationconcentrated under rotary evaporator
4. customAfter azeotropic removal of water with 1-propanol twice (20 mL each)
5. additionthe resulting solid was treated with methanol (5 mL)
6. additionethanol (12 mL) was added slowly
7. stirringstirred for additional 1 h
8. filtrationAfter filtration
9. customdrying of the resulting crystalline solid