反应详情

温度

100 °C

A mixture of 2,6-dichloro-3',4'-dimethoxy-2'-hydroxy-6'-methyl-benzophenone, potassium salt (1.13 g; 3 mmol), 1-bromobutane (0.69 g, 5 mmol) and dimethyl formamide (5 ml) are stirred at 100° C. for 8 h, and concentrated in vacuo. The residue is dissolved by shaking with a toluene/water mixture, after separation, the organic layer is collected washed with water and dried. After addition of silica gel (5 g), the solvent is evaporated. A flash chromatography column is packed with silica gel (25 g) and the charged silica gel is layered on top of that. Elution with petrol ether/ethyl acetate (95/5, 500 ml) gives the title compound, 0.82 g, (69% y) as colourless crystals, mp. 70° C.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue is dissolved
3. stirringby shaking with a toluene/water mixture
4. customafter separation
5. customthe organic layer is collected
6. washwashed with water
7. customdried
8. additionAfter addition of silica gel (5 g)
9. customthe solvent is evaporated
10. washElution with petrol ether/ethyl acetate (95/5, 500 ml)