HRID1679391

反应详情

EQUATION

反应方程式

HRID 1679391 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 25.4 g. 2-chloro-N-propylaniline and 15.15 g. dry triethylamine in 200 ml. dry ether was added to a solution of 13 ml. thiophosgene in 200 ml. of the same solvent at -20° C. The reaction mixture was allowed to warm to room temperature and then filtered, the filtered solid being washed with ether. The ethereal extract was added to the ethereal liquor and after drying over sodium sulphate, was evaporated to give a dark oil. On standing further solid precipitated, which was then separated from the oil. The oily filtrate was distilled to give the product N-2-chlorophenyl-N-propyl(thiocarbamoyl) chloride, b.p. 119°-120° C./0.4 mm. Hg.

WORKUP

后处理

  1. customat -20° C
  2. filtrationfiltered
  3. washthe filtered solid being washed with ether
  4. extractionThe ethereal extract
  5. additionwas added to the ethereal liquor
  6. dry with materialafter drying over sodium sulphate
  7. customwas evaporated
  8. customto give a dark oil
  9. customprecipitated
  10. customwhich was then separated from the oil
  11. distillationThe oily filtrate was distilled