HRID1959161

反应详情

EQUATION

反应方程式

HRID 1959161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Bis-(2,2,2-trifluoroethyl)phosphonoacetic acid (0.07 mol) was dissolved in 100 ml of ethyl acetate. To this solution 5.6 g of pyridine (0.07 mol) were added, followed by 20.4 g (0.093 mol) of Boc anhydride. The mixture was stirred for 15 min and anhydrous dimethylamine (0.07 mol) was added. The mixture was stirred overnight. The mixture was stirred for 1 h at 5° C., and worked-up. Following distillation bis(2,2,2-trifluoroethyl) 2-(dimethylamino)-2-oxoethylphosphonate was obtained in 80% yield.

WORKUP

后处理

  1. stirringThe mixture was stirred overnight
  2. stirringThe mixture was stirred for 1 h at 5° C.
  3. distillationdistillation bis(2,2,2-trifluoroethyl) 2-(dimethylamino)-2-oxoethylphosphonate
  4. customwas obtained in 80% yield