HRID1511453

反应详情

EQUATION

反应方程式

HRID 1511453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customat −78° C.
  2. customthe reaction mixture was quenched
  3. additionby slowly adding 1N HCl (15 mL)
  4. additionafter the addition
  5. additionThe reaction mixture was diluted with ethyl acetate (500 mL)
  6. washwashed with 1N HCl, water
  7. dry with materialbrine, and dried over magnesium sulfate
  8. customRemoval of the solvents under reduced pressure