HRID1902894

反应详情

EQUATION

反应方程式

HRID 1902894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Pentafluoroaniline (17 g, 0.106 mol) is dissolved in 300 ml of toluene with heating. The 2-carbethoxyhydrazinecarbonyl chloride, 19.4 g (0.122 M) is added to the hot solution. The mixture is refluxed until a white solid precipitates. The solid is filtered to give 24.8 g. The product is crystallized by dissolving in ethyl acetate/toluene (1/2 by vol) and evaporating until crystals appear, mp 180°-182°.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureThe mixture is refluxed until a white solid
  3. customprecipitates
  4. filtrationThe solid is filtered
  5. customto give 24.8 g
  6. customThe product is crystallized
  7. dissolutionby dissolving in ethyl acetate/toluene (1/2 by vol)
  8. customevaporating until crystals