反应详情

温度

5 °C

To a mixture of 3.9 g of AlCl3 and 4.67 g of 2,3-dichloroanisole in 70 ml of 1,2-dichloroethane at -10° C., 5 g of o-methoxybenzoyl chloride is added dropwise. The mixture is stirred for 2.5 hours and is gradually warmed to 5° C. The reaction mixture is poured into concentrated HCl and ice. The mixture is stirred one half hour to decompose the complex. The aqueous layer is extracted with additional organic solvent. The combined organic layers are washed until neutral, dried over Na2SO4 and evaporated to give an oil which solidifies on trituration with hexane. The crude product is recrystallized from 95% ethanol giving 2,3-dichloro-2',4-dimethoxybenzophenone, mp 94°-96° C.

1. stirringThe mixture is stirred one half hour
2. extractionThe aqueous layer is extracted with additional organic solvent
3. washThe combined organic layers are washed until neutral,
4. dry with materialdried over Na2SO4
5. customevaporated
6. customto give an oil which
7. customThe crude product is recrystallized from 95% ethanol