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温度

0 °C

Aluminum chloride (14.67 g, 0.1 mol), 2,6-dichlorobenzoyl chloride (20.95 g, 0.1 mol) and a solution of 3,4,5-trimethoxytoluene (18.22 g, 0.1 mol) in dichloromethane (50 ml), are slowly and consecutively added to dichloromethane stirred at 0° C., stirred for 1 h at ice bath temperatures and for 16 h at room temperature, and poured into ice. The organic layer is separated, washed with dilute hydrochloric acid and water, dried, and, after addition of silica gel (100 g), concentrated in vacuo. A flash chromatography column is packed with silica gel (400 g) andthe charged silica gel is layered on top of that. Elution with petrol ether/ethyl acetate (90/10, 1 l; 80/20, 1 l; 50/50, 1 l) yields 2,6-dichloro-3',4'-dimethoxy-2'-hydroxy-6'-methylbenzophenone, 10.35 g, (30% y), mp. 161° C.

1. stirringstirred for 1 h at ice bath temperatures
2. additionpoured into ice
3. customThe organic layer is separated
4. washwashed with dilute hydrochloric acid and water
5. customdried
6. additionafter addition of silica gel (100 g)
7. concentrationconcentrated in vacuo
8. washElution with petrol ether/ethyl acetate (90/10, 1 l; 80/20, 1 l; 50/50, 1 l)