HRID1248954

反应详情

EQUATION

反应方程式

HRID 1248954 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 m-aminobenzoate was dissolved in 500 ml of toluene and to the solution was added dropwise 83.4 g of N,N-diethylthiocarbamoyl chloride at room temperature with stirring over a period of about 1 hour. The mixture was then refluxed by heating for 5 hours. The toluene was distilled off under reduced pressure, to the residue was added 300 ml of ethyl acetate and the ethyl acetate solution was washed with water. The ethyl acetate was distilled off under reduced pressure and the residue was further subjected to vacuum distillation to obtain 80 g of ethyl m-isothiocyanatobenzoate as oily product. Boiling Point: 125° C./0.6 mm Hg. Yield: 77%.

WORKUP

后处理

  1. temperatureThe mixture was then refluxed
  2. temperatureby heating for 5 hours
  3. distillationThe toluene was distilled off under reduced pressure, to the residue
  4. additionwas added 300 ml of ethyl acetate
  5. washthe ethyl acetate solution was washed with water
  6. distillationThe ethyl acetate was distilled off under reduced pressure
  7. distillationthe residue was further subjected to vacuum distillation