HRID53954

反应详情

EQUATION

反应方程式

HRID 53954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

28.0 g of 5-bromo-2-methylbenzothiazole was dissolved in 200 ml of N-methyl-2-pyrrolidone, the solution thus prepared was mixed with 13.8 g of cuprous cyanide and a catalytically effective amount of copper sulfate, and the mixture was stirred for 4 hours with heating at a temperature of 180° to 190° C. in a stream of nitrogen. The resulting reaction solution was poured into water, and insoluble materials thus formed were collected by filtration. The thus collected insoluble materials were mixed with a mixture consisting of 22 ml of methylenediamine and 50 ml of water, and the resulting mixture was stirred thoroughly. After extraction with benzene, the resulting organic layer was washed with water, and dried to distill of benzene. Thereafter, the residue thus formed was washed with ethanol to obtain 10.22 g of 2-methyl-5-benzothiazolecarbonitrile in the form of light brown crystals.

WORKUP

后处理

  1. customthe solution thus prepared
  2. temperaturewith heating at a temperature of 180° to 190° C. in a stream of nitrogen
  3. customThe resulting reaction solution
  4. customthus formed
  5. filtrationwere collected by filtration
  6. additionThe thus collected insoluble materials were mixed with a mixture
  7. extractionAfter extraction with benzene
  8. washthe resulting organic layer was washed with water
  9. customdried
  10. distillationto distill of benzene
  11. customThereafter, the residue thus formed
  12. washwas washed with ethanol