反应详情

Methyl 2-(5-acetyl-2-benzyloxyphenyl)acetate (9.0 g), 18 ml of methyl orthoformate and 18 ml of ethylene glycol were dissolved in 300 ml of methylene chloride, 60 mg of p-toluenesulfonic acid monohydrate was added to the solution, and the mixture was heated under reflux for 12 hours. After cooling, 0.14 ml of triethylamine was added to the reaction solution and the mixture was stirred for 15 minutes. The reaction solution was partially purified by silica gel flash column chromatography (eluent: methylene chloride) and then further purified by silica gel medium pressure liquid column chromatography (eluent: hexane/diethyl ether=3/2) to give 9.2 g of methyl 2-[2-benzyloxy-5-(2-methyl-1,3-dioxolan-2-yl)phenyl]acetate in an oily form.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 12 hours
3. temperatureAfter cooling
4. customThe reaction solution was partially purified by silica gel flash column chromatography (eluent: methylene chloride)
5. customfurther purified by silica gel medium pressure liquid column chromatography (eluent: hexane/diethyl ether=3/2)