HRID615205

反应详情

EQUATION

反应方程式

HRID 615205 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.0 g of 2,6-difluorobenzoyl isocyanate in 15 ml of dry methylene chloride was added to a stirred solution of 3.1 g of 1,1,1-trichloro-N-[4-(trifluoromethyl)phenyl]methanesulphenamide in 35 ml of the same solvent at room temperature. After 2 days, only partial reaction had occurred and 2.0 g of the isocyanate was added. After a total reaction time of 28 days, the reaction mixture was diluted with 400 ml of light petroleum (b.p. 40°-60° C.) and filtered. Evaporation of the solvent from the filtrate gave a residue from which 6 was obtained as colorless crystals, m.p.: 129°-130° C., by chromatography on silica gel using methylene chloride as eluent.

WORKUP

后处理

  1. customonly partial reaction
  2. filtrationfiltered
  3. customEvaporation of the solvent from the filtrate
  4. customgave a residue from which 6
  5. customwas obtained as colorless crystals, m.p.: 129°-130° C., by chromatography on silica gel