HRID967156

反应详情

EQUATION

反应方程式

HRID 967156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of trans-3-{4-[2-(tert-butoxycarbonyl-methyl-amino)-ethyl]-cyclohexyl}-propionic acid ethyl ester in 40 ml of tetrahydrofuran was added under ice-cooling 547 mg (14.0 mmol) of lithium aluminium hydride in small portions. The reaction mixture was then stirred for 1 hour at room temperature. To destroy the excess of lithium aluminium hydride, 50 ml of brine was added to the reaction mixture under ice-cooling. It was then partitioned between ether and water, the organic layer was dried over magnesium sulfate and concentrated under reduced pressure giving 3.35 g (100% over 2 stepts) nearly pure trans-{2-[4-(3-hydroxy-propyl)-cyclohexyl]-ethyl}-methyl-carbamic acid tert-butyl ester as colorless viscous oil, MS. 317 (MNH4+).

WORKUP

后处理

  1. customTo destroy the excess of lithium aluminium hydride, 50 ml of brine
  2. additionwas added to the reaction mixture under ice-
  3. temperaturecooling
  4. customIt was then partitioned between ether and water
  5. dry with materialthe organic layer was dried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure