反应详情

20 g of 2-methoxy-1,3-propanediol was dissolved in 200 ml of pyridine. 52.6 ml of phenyl chlorocarbonate was added dropwise to the solution under stirring and under cooling with ice. After two hours, the reaction solution was added to 1 l of 4 N hydrochloric acid/water. After extraction with ether, the organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate, concentrated and purified according to silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1) to obtain 52 g of the intended product.

1. temperatureunder cooling with ice
2. extractionAfter extraction with ether
3. washthe organic layer was washed with a saturated aqueous solution of sodium hydrogencarbonate
4. concentrationconcentrated
5. custompurified