Water → 1,3-Dioxepin, 2-(1,1-dimethylethyl)-4,7-dihydro-

HRID 34428

반응식

HRID 34428 반응식
[CH3:1][C:2]([CH3:6])([CH3:5])[CH:3]=[O:4].[CH2:7](O)[CH:8]=[CH:9][CH2:10][OH:11].O>C1(C)C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:2]([CH:3]1[O:11][CH2:10][CH:9]=[CH:8][CH2:7][O:4]1)([CH3:6])([CH3:5])[CH3:1]

참가 물질

6

반응물 3

HCID 962WaterHCID 80652-Butene-1,4-diolHCID 12417Pivalaldehyde

생성물 1

HCID 110626301,3-Dioxepin, 2-(1,1-dimethylethyl)-4,7-dihydro-수율 89.9%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 1140Toluene용매

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d179930b3754451789634e378a8dd266
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04761489

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