HRID1434930

反应详情

EQUATION

反应方程式

HRID 1434930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,2-dimethyl-3-thiophen-2-yl-propionic acid (315 mg, 1.589 mmol) in 10 ml of dichloromethane was treated successively with HOBt (257 mg, 1.9 mmol), EDC (364 mg, 1.9 mmol) and triethylamine (0.223 ml, 1.6 mmol). The mixture was stirred for 20 minutes, then methylamine (0.621 ml, 8 mmol) was added and stirring was continued for 18 hours. The solvent was then evaporated and the crude was redissolved in ether, washed with 2N-HCl, saturated sodium bicarbonate and brine. Drying over sodium sulfate and evaporation gave a yellow-brown oil which was used without further purification. Yield: 244 mg (78%).

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 18 hours
  3. customThe solvent was then evaporated
  4. dissolutionthe crude was redissolved in ether
  5. washwashed with 2N-HCl, saturated sodium bicarbonate and brine
  6. dry with materialDrying over sodium sulfate and evaporation
  7. customgave a yellow-brown oil which
  8. customwas used without further purification