HRID875334

反应详情

EQUATION

反应方程式

HRID 875334 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Under reflux, 45 ml of a 3.5 M solution of lithium aluminium hydride in toluene were slowly added dropwise to a solution of 35.4 g (136.98 mmol) of methyl 4-[2-(4-fluorophenyl)ethyl]benzoate in 500 ml of dry THF. After the addition had ended, the reaction mixture was stirred under reflux for one hour. The reaction mixture was then cooled to 0° C., and 500 ml of ice-cooled 1 M hydrochloric acid were added slowly and carefully. 750 ml of ethyl acetate were then added, the aqueous phase was removed and the organic phase was washed successively in each case once with 1 M hydrochloric acid and saturated sodium chloride solution. The organic phase was then dried over magnesium sulphate, filtered and concentrated to dryness. This gave 31.5 g (136.7 mmol, 99.9% of theory) of the title compound.

WORKUP

后处理

  1. temperatureUnder reflux
  2. additionAfter the addition
  3. temperatureunder reflux for one hour
  4. additionwere added slowly
  5. customthe aqueous phase was removed
  6. washthe organic phase was washed successively in each case once with 1 M hydrochloric acid and saturated sodium chloride solution
  7. dry with materialThe organic phase was then dried over magnesium sulphate
  8. filtrationfiltered
  9. concentrationconcentrated to dryness