1,2-Dichloroethane → 1,1'-Dimethyl 2,2'-oxybis(acetate)

HRID 37053

반응식

HRID 37053 반응식
[C:1]([OH:9])(=[O:8])[CH2:2][O:3][CH2:4][C:5]([OH:7])=O.[CH3:10][OH:11].Cl[CH2:13]CCl>>[CH3:10][O:11][C:5](=[O:7])[CH2:4][O:3][CH2:2][C:1]([O:9][CH3:13])=[O:8]

참가 물질

4

반응물 3

HCID 111,2-DichloroethaneHCID 887MethanolHCID 8088Diglycolic Acid

생성물 1

HCID 2018771,1'-Dimethyl 2,2'-oxybis(acetate)

실험 절차

Diglycolic acid (67.05 g, 0.5 mol) was dissolved in a mixture of methanol (122 ml, 30 mol) and 1,2-dichloroethane (150 ml). KSF-catalyst (Aldrich) (2.5 g) was added and the mixture was refluxed for 15 hours. The mixture was cooled to ambient temperature, filtered through alumina, washed with aqueous saturated sodium hydrogen carbonate (100 ml) and dried over magnesium sulphate. The solvent was evaporated and diglycolic acid dimethyl ester was isolated after distillation as a colourless oil. Yield 39.5 g (49%) b.p. 65°-66° C. (0.055 mmHg).

후처리

  1. additionKSF-catalyst (Aldrich) (2.5 g) was added
  2. temperaturethe mixture was refluxed for 15 hours
  3. filtrationfiltered through alumina
  4. washwashed with aqueous saturated sodium hydrogen carbonate (100 ml)
  5. dry with materialdried over magnesium sulphate
  6. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-923b1537a8f547878e110fc8e786586e
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05419893

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