HRID1707528

反应详情

EQUATION

反应方程式

HRID 1707528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

340 cm] (1.3 mol) of a 70% NaAlH2 (OC2H4OCH3)2 in toluene with 340 cm3 of anhydrous toluene was stirred at room temperature while adding 57 g (0.2 mol) of diethyl 4-propylcyclohexylmalonate dropwise for 30 minutes, after which it was stirred for 5 hours on a hot water bath at 80°-90° C. The reactant was cooled to room temperature, and 50 cm3 of water and 1,000 cm3 of 15% HCl were dropped while stirring. The oily layer was removed, and the water layer was extracted with toluene and combined with the oily layer and washed with 10% HC1 and water. The toluene was removed, and the residue was recrystallized from hexane to obtain 18 g (0.09 mol) of 2-(4'-propylcyclohexyl)propane-1,3-diol (trans-cis form mixture).

WORKUP

后处理

  1. stirringwhile stirring
  2. customThe oily layer was removed
  3. extractionthe water layer was extracted with toluene
  4. washwashed with 10% HC1 and water
  5. customThe toluene was removed
  6. customthe residue was recrystallized from hexane