反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 2.5 g (0.006 mole) sodium borohydride in 30 ml of absolute ethanol was added dropwise 30 ml of an absolute ethanol solution containing 3.5 g 80.0135 mole) of the ethyl 5-hydroxy-3-oxo-6-phenoxyheptanoate obtained in step (a). After completion of the addition, cooling was immediately stopped and the mixture was allowed to warm to room temperature and was stirred for about 40 minutes. To the reaction mixture were then added about 300 ml of ice-water and the mixture was then acidified by the addition of 2 N sulphuric acid. After saturating the solution with sodium chloride, it was extracted three times, each time with 50 ml of ethyl acetate. The combined extracts were dried over anhydrous sodium sulphate and then the solvent was evaporated off, to give 1.3 g (yield 37%) of ethyl 3,5-dihydroxy-6-phenoxyheptanoate.
WORKUP
后处理
- additionAfter completion of the addition
- temperaturecooling
- concentrationAfter saturating the solution with sodium chloride, it
- extractionwas extracted three times
- dry with materialThe combined extracts were dried over anhydrous sodium sulphate
- customthe solvent was evaporated off