HRID845371

反应详情

EQUATION

反应方程式

HRID 845371 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

128 g (4 moles) of methanol and 2 g (0.05 mole) of NaOH were initially taken under nitrogen in a reaction flask and were refluxed. A mixture of 142 g (1 mole) of 3,5,5-trimethylhexanal and 116 g (2 moles) of propionaldehyde was added dropwise to this solution in the course of 10 minutes. The resulting reaction mixture was kept at the boil for 1 hour (h) and then brought to pH 4-5 with an 80% strength aqueous acetic acid solution. After washing twice with water, the organic phase was separated off and worked up by fractional distillation. 32 g of unconverted 3,5,5-trimethylhexanal, as light ends, and 113 g of 2,5,7,7-tetramethyl-2-octenal (bp.=108°-111° C./14 mbar) were obtained, corresponding to a selectivity of 81%, based on trimethylhexanal; nD25 =1.4580.

WORKUP

后处理

  1. temperaturewere refluxed
  2. additionwas added dropwise to this solution in the course of 10 minutes
  3. customThe resulting reaction mixture
  4. washAfter washing twice with water
  5. customthe organic phase was separated off
  6. distillationworked up by fractional distillation