HRID870672

反应详情

EQUATION

反应方程式

HRID 870672 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a rapidly stirred, 0° C., N2 blanketed, solution of 2,2,2-trifluoro-N-(3-methylamino-propyl)-acetamide (6.0 g, 32.4 mmol) and N-methylmorpholine [109-02-4] (7.1 mL, 64.6 mmol) in ethyl acetate (65 mL) was steadily added a 1.0M solution of isopropyl chloroformate in toluene (32.4 mL) over the course of 10 minutes. The reaction was allowed to stir and warm to ambient temperature over night at which time it was washed with brine, dried (MgSO4) and evaporated to provide 9.0 g of clear yellow oil. LRMS (ESI) m/z 271.1 [(M+H)]+, calc'd for C10H17F3N2O3: 270.25.

WORKUP

后处理

  1. stirringto stir
  2. temperaturewarm to ambient temperature over night at which time it
  3. washwas washed with brine
  4. dry with materialdried (MgSO4)
  5. customevaporated