反应详情

温度

-10 °C

N-(t-Butyloxy)-2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3(R)-(3-picolyloxy)butanamide (1.3 g, 2.4 mmol) is dissolved in methylene chloride (50 mL) containing ethanol (0.14 mL, 2.4 mmol) in a round bottom flask, and the reaction is cooled to -10° C. Hydrochloric acid gas (from a lecture bottle) is bubbled through for 20 minutes. The reaction is sealed, allowed to slowly warm to room temperature, and stirred for two days. The solvent is reduced to 1/3 the volume by evaporation and the residue is triturated with ether. The mixture is filtered, the fiter cake is removed and dried in vacuo to provide N-hydroxy-2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3(R)-(3-picolyloxy)-butanamide dihydrochloride as a white solid; [α]D25 =+35.26° (c=5.58, DMSO).

1. customHydrochloric acid gas (from a lecture bottle) is bubbled through for 20 minutes
2. customThe reaction is sealed
3. temperatureto slowly warm to room temperature
4. customby evaporation
5. customthe residue is triturated with ether
6. filtrationThe mixture is filtered
7. customthe fiter cake is removed
8. customdried in vacuo