HRID26433

反应详情

EQUATION

反应方程式

HRID 26433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 156.9 g. of 1-(2,6-dichlorophenyl)thiourea in 1 l. of chlorobenzene was refluxed for 20 hours and concentrated. The resulting oil was triturated with 1 l. of hot hexane which was filtered. On cooling overnight, 52 g. (36%) of 2,6-dichlorophenylisothiocyanate, m.p. 41°-42° separated. Concentration of the filtrate gave an additional 64.2 g. (44%), m.p. 41°-43° in two crops. Recrystallization of a sample from hexane gave the analytical sample, m.p. 41°-42°.

WORKUP

后处理

  1. concentrationconcentrated
  2. customThe resulting oil was triturated with 1 l
  3. filtrationof hot hexane which was filtered
  4. temperatureOn cooling overnight
  5. custom(36%) of 2,6-dichlorophenylisothiocyanate, m.p. 41°-42° separated
  6. customConcentration of the filtrate gave an additional 64.2 g
  7. customRecrystallization of a sample from hexane
  8. customgave the analytical sample, m.p. 41°-42°