反应 #62706

反应方程式

2,2-dimethylpropanal

but-2-ene-1,4-diol

water

→

2-tert-butyl-4,7-dihydro-1,3-dioxepin

收率 89.9%

溶剂

toluene

反应条件

后处理

1. 1
   温度was refluxed
2. 2
   其他formed
3. 3
   其他was removed in the course of 3 hours (h)
4. 4
   workup.WAITThe mixture was then left
5. 5
   workup.ADDITION10 ml of a 25% strength sodium hydroxide solution were added to the solution
6. 6
   洗涤the mixture was washed neutral with a little water
7. 7
   workup.DISTILLATIONthe toluene was distilled off under reduced pressure at from 50° to 60° C
8. 8
   其他The residue obtained
9. 9
   workup.DISTILLATIONwas distilled under 0.1 mbar

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.

来源