HRID1511453
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To the solution of (S)-tert-butyl 3-cyclobutyl-1-(methoxy(methyl)amino)-1-oxopropan-2-ylcarbamate (4.3 g, 15 mmol) in anhydrous tetrahydrofuran (100 mL) under argon at −78° C., was slowly added lithium aluminum hydride (1M in tetrahydrofuran, 15 mL, 15 mmol). After 2 hours, the reaction mixture was quenched by slowly adding 1N HCl (15 mL) and the reaction mixture was warmed up to room temperature after the addition was complete. The reaction mixture was diluted with ethyl acetate (500 mL), washed with 1N HCl, water, then brine, and dried over magnesium sulfate. Removal of the solvents under reduced pressure gave (S)-tert-butyl 1-cyclobutyl-3-oxopropan-2-ylcarbamate (2.95 g) as an oil.
WORKUP
后处理
- customat −78° C.
- customthe reaction mixture was quenched
- additionby slowly adding 1N HCl (15 mL)
- additionafter the addition
- additionThe reaction mixture was diluted with ethyl acetate (500 mL)
- washwashed with 1N HCl, water
- dry with materialbrine, and dried over magnesium sulfate
- customRemoval of the solvents under reduced pressure