HRID1751170

反应详情

EQUATION

反应方程式

HRID 1751170 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

57 g (0.25 mol) of 2-[1-(3,3-dimethyl-cyclohexyl)-ethoxy]-2-methyl-propan-1-ol, 41.6 g (0.4 mol) of methoxyacetic acid methyl ester and 0.3 g of sodium methylate in 50 g methanol were placed in a 250-ml stirred vessel and were boiled under reflux. During this, methanol was distilled off via a still head. Then 100 ml water and 100 ml toluene were added to the reaction solution at room temperature, the aqueous phase was separated, the organic phase was washed with water until neutral and concentrated by evaporation. The raw product (81 g) was fractionated on a 30-cm Vigreux column in vacuum.

WORKUP

后处理

  1. temperatureunder reflux
  2. distillationDuring this, methanol was distilled off via a still head
  3. additionThen 100 ml water and 100 ml toluene were added to the reaction solution at room temperature
  4. customthe aqueous phase was separated
  5. washthe organic phase was washed with water until neutral and
  6. concentrationconcentrated by evaporation