反应详情

温度

95 °C

A solution of 2-(3,4-dichlorophenyl)-2-methylpropionitrile (12.8 g) in ether (100 ml) was added dropwise at −10° C. under nitrogen over 20 minutes to stirred ethereal methylmagnesium iodide solution (3M; 30 ml), then the mixture was stirred at reflux temperature for 2 hour and at ambient temperature for 18 hours. The resulting solid was collected by filtration, washed well with ether, and added in portions to a mixture of ice-cold water (100 ml) and concentrated hydrochloric acid (50 ml). The resulting mixture was heated at 95° C. with occasional stirring for 1 hour, then cooled to ambient temperature. The product was extracted into dichloromethane (3×100 ml), then the combined extracts were dried (CaCl2), and the solvents were removed in vacuo to give 3-(3,4-dichlorophenyl)-3-methylbutan-2-one as a pale brown oil (9.07 g) which was used without further purification.

1. temperatureat reflux temperature for 2 hour
2. filtrationThe resulting solid was collected by filtration
3. washwashed well with ether
4. additionadded in portions to a mixture of ice-cold water (100 ml) and concentrated hydrochloric acid (50 ml)
5. stirringwith occasional stirring for 1 hour
6. temperaturecooled to ambient temperature
7. extractionThe product was extracted into dichloromethane (3×100 ml)
8. dry with materialthe combined extracts were dried (CaCl2)
9. customthe solvents were removed in vacuo