HRID1912228

反应详情

EQUATION

反应方程式

HRID 1912228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customIn a 50 ml three-necked flask equipped with a condenser
  2. customThe precipitate formed
  3. filtrationwas filtered off
  4. extractionextracted with ethyl acetate (3×30 ml)
  5. dry with materialThe organic phase was dried over sodium sulphate
  6. filtrationfiltered
  7. filtrationon filter paper
  8. concentrationconcentrated
  9. customThe colourless oil obtained
  10. customwas purified by chromatography on silica gel (eluent: dichloromethane/methanol)
  11. customThe colourless oil obtained
  12. customwas dried under vacuum