HRID1192962

反应详情

EQUATION

反应方程式

HRID 1192962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Amino-4,4,4-trifluoro-2-methyl-but-2-enoic acid ethyl ester (25.5 g, 124 mmol) was cooled to 0° C. and methyl hydrazine (7 ml, 132 mmol) was added dropwise. The mixture was allowed to warm to room temperature and heated to 50° C. for 20 hours. The mixture was allowed to cool to room temperature and was stirred for 16 hours. The mixture was cooled to 0° C. and saturated aqueous sodium hydrogencarbonate solution (50 ml) was added. The solid was removed by filtration and washed with cold water (0° C.) to give the product as a white solid (8.46 g, 38% yield over two steps).

WORKUP

后处理

  1. temperatureheated to 50° C. for 20 hours
  2. temperatureto cool to room temperature
  3. temperatureThe mixture was cooled to 0° C.
  4. customThe solid was removed by filtration
  5. washwashed with cold water (0° C.)