HRID34428

反应详情

EQUATION

反应方程式

HRID 34428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 430 g (5 moles) of 2,2-dimethylpropanal, 3 g of p-toluenesulfonic acid and 440 g (5 moles) of but-2-ene-1,4-diol in 1000 ml of toluene was refluxed, and the water of reaction formed was removed in the course of 3 hours (h). The mixture was then left to cool to room temperature, 10 ml of a 25% strength sodium hydroxide solution were added to the solution, the mixture was washed neutral with a little water and the toluene was distilled off under reduced pressure at from 50° to 60° C. The residue obtained was distilled under 0.1 mbar to give 702 g of 2-tert-butyl-4,7-dihydro-1,3-dioxepin of boiling point 80° C./32 mbar.

WORKUP

后处理

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