HRID34430

反应详情

EQUATION

反应方程式

HRID 34430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 720 g (5 moles) of 2,5-dimethylhex-3-ene-2,5-diol, 3 g of p-toluenesulfonic acid, 500 g (5 moles) of n-hexanal and 1 l of toluene was refluxed, and the resulting water of reaction (115 ml) was separated off in the course of 5.5 h. The mixture was then left to cool, 10 ml of a 25% strength aqueous sodium hydroxide solution were added, the mixture was washed neutral with a little water and the toluene was removed under reduced pressure at from 50° to 60° C. The residue obtained was distilled under 0.1 mbar to give 796 g of 2-pentyl-4,4,7,7-tetramethyl-4,7-dihydro-1,3-dioxepin of boiling point 75° C./0.1 mbar.

WORKUP

后处理

  1. temperaturewas refluxed
  2. customwas separated off in the course of 5.5 h
  3. waitThe mixture was then left
  4. temperatureto cool
  5. addition10 ml of a 25% strength aqueous sodium hydroxide solution were added
  6. washthe mixture was washed neutral with a little water
  7. customthe toluene was removed under reduced pressure at from 50° to 60° C
  8. customThe residue obtained
  9. distillationwas distilled under 0.1 mbar