Ethylene Glycol → Methyl 4,4-ethylenedioxy-3-methyl-butanoate

HRID 27353노트

반응식

HRID 27353 반응식
[CH3:1][CH:2]([CH:8]=[O:9])[CH2:3][C:4]([O:6][CH3:7])=[O:5].[CH2:10](O)[CH2:11][OH:12].C1(C)C=CC(S(O)(=O)=O)=CC=1.C1C=CC=CC=1>CCOCC>[CH2:10]1[CH2:11][O:12][CH:8]([CH:2]([CH3:1])[CH2:3][C:4]([O:6][CH3:7])=[O:5])[O:9]1

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 241BenzeneHCID 6101p-Toluenesulfonic acidHCID 11804788Methyl 3-methyl-4-oxobutanoate

생성물 1

HCID 20305753Methyl 4,4-ethylenedioxy-3-methyl-butanoate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of methyl 3-methyl-4-oxo-butanoate (86.3 g), ethylene glycol (61.75 l g, 0.996 m), p-toluenesulfonic acid (1 g) and benzene (700 ml) is refluxed under nitrogen for 16 hr. The resulting mixture is allowed to cool to room temperature and treated with ether (300 ml). The organic phase is washed with 5% sodium bicarbonate solution (100 ml), dried (Na2SO4) and evaporated in vacuo to give methyl 4,4-ethylenedioxy-3-methylbutanoate as a crude product (63.2 g). This material is used directly in the next step.

후처리

  1. temperatureis refluxed under nitrogen for 16 hr
  2. washThe organic phase is washed with 5% sodium bicarbonate solution (100 ml)
  3. dry with materialdried (Na2SO4)
  4. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-a33fd6e19fd54f87b28e349a7fcd51ce
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04221717

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