반응 #62706

반응 방정식

2,2-dimethylpropanal

but-2-ene-1,4-diol

water

→

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

수율 89.9%

용매

toluene

반응 조건

후처리

1. 1
   온도was refluxed
2. 2
   기타formed
3. 3
   기타was 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
   세척the 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
   기타The residue obtained
9. 9
   workup.DISTILLATIONwas distilled under 0.1 mbar

실험 절차

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.

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