反应详情

温度

47.5 °C

A solution of 86.2 g (5-bromo-2-chloro-phenyl)-(4-methoxy-phenyl)-methanone and 101.5 ml triethylsilane in 75 ml dichloromethane and 150 ml acetonitrile is cooled to 10° C. Then with stirring 50.8 ml of boron trifluoride etherate are added so that the temperature does not exceed 20° C. The solution is stirred for 14 h at ambient temperature, before another 9 ml triethylsilane and 4.4 ml boron trifluoride etherate are added. The solution is stirred for a further 3 h at 45-50° C. and then cooled to ambient temperature. A solution of 28 g potassium hydroxide in 70 ml of water is added and the mixture is stirred for 2 h. Then the organic phase is separated off and the aqueous phase is extracted another three times with diisopropylether. The combined organic phases are washed twice with 2 M potassium hydroxide solution and once with aqueous sodium chloride solution and then dried over sodium sulfate. After the solvent is removed the residue is washed with ethanol and dried at 60° C.

1. additionare added so that the temperature
2. customdoes not exceed 20° C
3. additionare added
4. temperaturecooled to ambient temperature
5. stirringthe mixture is stirred for 2 h
6. customThen the organic phase is separated off
7. extractionthe aqueous phase is extracted another three times with diisopropylether
8. washThe combined organic phases are washed twice with 2 M potassium hydroxide solution and once with aqueous sodium chloride solution
9. dry with materialdried over sodium sulfate
10. customAfter the solvent is removed the residue
11. washis washed with ethanol
12. customdried at 60° C.