HRID65476

反应详情

EQUATION

反应方程式

HRID 65476 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of 2.5 g (0.05 mol) of sodium hydride in a mixture of 40 ml of dry-dimethylacetamide and 40 ml of dry benzene, 0.05 mole of N-(2,6-dimethylphenyl)acetamide was added. After evolution of hydrogen ceased, the mixture was cooled in ice and water, and with stirring 0.075 mole of carbon disulfide was added slowly. The mixture was stirred at room temperature for 20 minutes. The reaction mixture was poured into water and extracted with toluene. The organic layer, dried over sodium sulfate, was evaporated, and distillation of the residue yielded 6.1 g (74%) of 2,6-dimethylphenylisothiocyanate.

WORKUP

后处理

  1. additionin a mixture of 40 ml
  2. additionwas added
  3. temperaturethe mixture was cooled in ice
  4. additionwas added slowly
  5. extractionextracted with toluene
  6. dry with materialThe organic layer, dried over sodium sulfate
  7. customwas evaporated
  8. distillationdistillation of the residue