HRID1096254

反应详情

EQUATION

反应方程式

HRID 1096254 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-75 °C

PROCEDURE

实验过程

Lithium aluminum hydride solution (1 M in THF (0.46 mL, 0.46 mmol) was added dropwise at −30° C. to a solution of N-methoxy-N-methyl-3-[3-methyl-2-oxo-4-(3-trifluoromethoxy-phenyl)-piperazin-1-yl]-propionamide (180 mg, 0.46 mmol) in THF (10 mL). The reaction mixture was cooled to −75° C., then acetone (0.59 g, 10 mmol) and AcOH (44 mg, 0.93 mmol) were added dropwise. The reaction mixture was then partitioned between TBME and 1 M aq. KHSO4 solution. The organic layer was dried (MgSO4), filtered, and evaporated to afford the title compound (122 mg, 80%). Light yellow oil, MS: 331.1 (M+H)+.

WORKUP

后处理

  1. customThe reaction mixture was then partitioned between TBME and 1 M aq. KHSO4 solution
  2. dry with materialThe organic layer was dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated