HRID1094724

反应详情

EQUATION

反应方程式

HRID 1094724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2,2,2-trifluoroethylamine hydrochloride (0.5 g, 3.7 mmol) in MeOH (5 mL) was added triethylamine (0.51 mL, 0.37 mmol) followed by acetaldehyde (1.0 mL, excess). The reaction mixture was then stirred at 0° C. for 3 h. Sodium borohydride (1 g, 5.9 mmol) was then added and the reaction mixture was stirred at 0° C. for 20 min. The reaction was quenched with 1M NaOH (10 mL) and the aqueous layer was extracted with DCM (25 mL). The organic layer was separated and to it was added 2M HCl in Et2O (10 mL). The resultant precipitate was filtered to give 0.45 g of N-ethyl-2,2,2-trifluoroethanamine hydrochloride, (yield: 75%).

WORKUP

后处理

  1. stirringthe reaction mixture was stirred at 0° C. for 20 min
  2. customThe reaction was quenched with 1M NaOH (10 mL)
  3. extractionthe aqueous layer was extracted with DCM (25 mL)
  4. customThe organic layer was separated and to it
  5. additionwas added 2M HCl in Et2O (10 mL)
  6. filtrationThe resultant precipitate was filtered