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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
In a 50 ml three-necked flask equipped with a condenser, a thermometer and a magnetic stirrer, 1 g (4.5 mmol) of methyl (+/−)-jasmonate was dissolved in 15 ml of tetrahydrofuran. 430 mg (11.3 mmol) of lithium aluminium hydride, LiAlH4, were added. The mixture was stirred at 50° C. for 4 hours. When the reaction was finished, 5 ml of water were added slowly. The precipitate formed was filtered off and the filtrate was acidified to pH=5 with hydrochloric acid and then extracted with ethyl acetate (3×30 ml). The organic phase was dried over sodium sulphate, filtered on filter paper, and then concentrated. The colourless oil obtained was purified by chromatography on silica gel (eluent: dichloromethane/methanol). The colourless oil obtained was dried under vacuum.
WORKUP
后处理
- customIn a 50 ml three-necked flask equipped with a condenser
- customThe precipitate formed
- filtrationwas filtered off
- extractionextracted with ethyl acetate (3×30 ml)
- dry with materialThe organic phase was dried over sodium sulphate
- filtrationfiltered
- filtrationon filter paper
- concentrationconcentrated
- customThe colourless oil obtained
- customwas purified by chromatography on silica gel (eluent: dichloromethane/methanol)
- customThe colourless oil obtained
- customwas dried under vacuum