반응 #317813

반응 방정식

4-iodobenzonitrile

3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazole

N,N-dimethylglycine

cesium carbonate

→

title compound

수율 59.5%

4-[3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazol-1-yl]benzonitrile

수율 59.5%

용매

ethyl acetate

dimethylsulfoxide

반응 조건

후처리

1. 1
   여과Solid filtered off through kieselguhr
2. 2
   기타The filtrate was partitioned between ethyl acetate and water
3. 3
   기타The organic layer was separated
4. 4
   건조dried over sodium sulphate
5. 5
   기타The solvent was removed by rotary evaporation
6. 6
   기타triturated with diethyl ether

실험 절차

A mixture of 4-iodobenzonitrile (2.41 g, 10.5 mmol), 3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazole (2.0 g, 10.5 mmol), copper (I) oxide (20 mol %, 2.1 mmol, 300 mg), N,N-dimethylglycine (10.5 mmol, 1.082 g), and cesium carbonate (21 mmol, 6.84 g) in dimethylsulfoxide (5 ml) was heated in an oil bath at 130° C. under argon for 4 h. The reaction mixture was diluted with ethyl acetate. Solid filtered off through kieselguhr. The filtrate was partitioned between ethyl acetate and water. The organic layer was separated and dried over sodium sulphate. The solvent was removed by rotary evaporation and triturated with diethyl ether to give the title compound as a light brown solid (1.812 g, 59.5%).

출처