反応 #82232

反応方程式

5-bromo-2-methylbenzothiazole

N-methyl-2-pyrrolidone

water

→

2-methyl-5-benzothiazolecarbonitrile

反応条件

後処理

1. 1
   その他the solution thus prepared
2. 2
   温度with heating at a temperature of 180° to 190° C. in a stream of nitrogen
3. 3
   その他The resulting reaction solution
4. 4
   その他thus formed
5. 5
   ろ過were collected by filtration
6. 6
   workup.ADDITIONThe thus collected insoluble materials were mixed with a mixture
7. 7
   抽出After extraction with benzene
8. 8
   洗浄the resulting organic layer was washed with water
9. 9
   その他dried
10. 10
    workup.DISTILLATIONto distill of benzene
11. 11
    その他Thereafter, the residue thus formed
12. 12
    洗浄was washed with ethanol

実験手順

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.

出典