HRID1248958

反应详情

EQUATION

反应方程式

HRID 1248958 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

82.5 g of ethyl p-aminobenzoate was dissolved in 500 ml of toluene, to the solution was added 83.4 g of N,N-diethylthiocarbamoyl chloride and the mixture was refluxed by heating for 8 hours. After cooling with ice, 100 ml of concentrated hydrochloric acid was added to the reaction mixture and then the toluene layer was separated and washed with water. The toluene was distilled off under reduced pressure and the residual oily product was crystallized from methanol to obtain 77.1 g of ethyl p-isothiocyanatobenzoate. Yield: 74.5%. Melting Point: 52° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureby heating for 8 hours
  3. additionwas added to the reaction mixture
  4. customthe toluene layer was separated
  5. washwashed with water
  6. distillationThe toluene was distilled off under reduced pressure
  7. customthe residual oily product was crystallized from methanol