反应详情

温度

-10 °C

(a) N-(t-Butyloxy)-2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3-methylbutanamide (4.1 g, 9.13 mmol) is dissolved in dichloroethane (150 mL) containing ethanol (0.53 ml, 9.13 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 30 minutes. The reaction is sealed, allowed to slowly warm to room temperature, and stirred for 2 days. The solvent is reduced to 1/3 volume by evaporation and triturated with ether. The mixture is filtered, filter cake removed, and dried in vacuo to provide N-hydroxy-2(R)-[[4-methoxybenzenesulfonyl](3-picolyl)amino]-3-methylbutanamide hydrochloride as a white solid, m.p. 169°-170° C. (dec), and having the following structure: ##STR12##

1. customHydrochloric acid gas (from a lecture bottle) is bubbled through for 30 minutes
2. customThe reaction is sealed
3. temperatureto slowly warm to room temperature
4. customThe solvent is reduced to 1/3 volume by evaporation
5. customtriturated with ether
6. filtrationThe mixture is filtered
7. filtrationfilter cake
8. customremoved
9. customdried in vacuo