반응 #82232

반응 방정식

5-bromo-2-methylbenzothiazole

N-methyl-2-pyrrolidone

water

→

2-methyl-5-benzothiazolecarbonitrile

반응 조건

후처리

1. 1
   기타the solution thus prepared
2. 2
   온도with heating at a temperature of 180° to 190° C. in a stream of nitrogen
3. 3
   기타The resulting reaction solution
4. 4
   기타thus formed
5. 5
   여과were collected by filtration
6. 6
   workup.ADDITIONThe thus collected insoluble materials were mixed with a mixture
7. 7
   추출After extraction with benzene
8. 8
   세척the resulting organic layer was washed with water
9. 9
   기타dried
10. 10
    workup.DISTILLATIONto distill of benzene
11. 11
    기타Thereafter, the residue thus formed
12. 12
    세척was washed with ethanol

실험 절차

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.

출처