反应详情

Five grams of (2,4-dihydroxy-3-propylphenyl)- (2-hydroxyphenyl)methanone, 5.63 ml of triethylamine, and approximately 50 mg of dimethylaminopyridine were dissolved in 50 ml of diethyl ether at 0° C. Acetic anhydride (3.8 ml) was added dropwise. After stirring for 1 hour, the reaction mixture was partitioned between diethyl ether and water. The organic layer was separated, washed with 1N hydrochloric acid, a saturated solution of sodium bicarbonate, and a saturated solution of sodium chloride, dried over magnesium sulfate, and concentrated in vacuo. Purification by high pressure liquid chromatography over silica gel eluting with a 10-25% ethyl acetate in hexane gradient and concentration of the appropriate fractions provided 2.6 g of the desired title product as an oil.

1. customthe reaction mixture was partitioned between diethyl ether and water
2. customThe organic layer was separated
3. washwashed with 1N hydrochloric acid
4. dry with materiala saturated solution of sodium bicarbonate, and a saturated solution of sodium chloride, dried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. customPurification by high pressure liquid chromatography over silica gel eluting with a 10-25% ethyl acetate in hexane gradient and concentration of the appropriate fractions