HRID1655761

反应详情

EQUATION

反应方程式

HRID 1655761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

10.5 g (0.277 mol) of lithium aluminium hydride were suspended in 100 ml of absolute ether and treated while stirring within 10 minutes with 100 ml of absolute tetrahydrofuran. To this stirred suspension was added dropwise within 6-8 hours, while heating to reflux, 46.7 g (0.277 mol) of (+) 2-(2-furyl)-3-methylbutyric acid in 100 ml of absolute tetrahydrofuran. The reaction mixture was cooled and treated slowly with a 3N hydrochloric acid solution. The organic phase was separated, washed with water, dried and evaporated under reduced pressure. The remaining oil was distilled in a high vacuum, to obtain 32 g (75%) of (R)-(+)-2-(2-furyl)-3-methyl-1-butanol as a colorless liquid of 96% purity, boiling point 58°/39 Pa, [α]D20 =+2.5° (c=1%, ethanol).

WORKUP

后处理

  1. additiontreated
  2. additionTo this stirred suspension was added dropwise within 6-8 hours
  3. temperaturewhile heating
  4. temperatureto reflux
  5. temperatureThe reaction mixture was cooled
  6. customThe organic phase was separated
  7. washwashed with water
  8. customdried
  9. customevaporated under reduced pressure
  10. distillationThe remaining oil was distilled in a high vacuum