1,2-Dichloroethane → 1,1'-Dimethyl 2,2'-oxybis(acetate)
反応式
[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]参加物
4
実験手順
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.
後処理
- additionKSF-catalyst (Aldrich) (2.5 g) was added
- temperaturethe mixture was refluxed for 15 hours
- filtrationfiltered through alumina
- washwashed with aqueous saturated sodium hydrogen carbonate (100 ml)
- dry with materialdried over magnesium sulphate
- customThe solvent was evaporated
出典と根拠
- ORDレコード
- ord-0511df2ffccf40bc98e811058e3432a5
- 出典データセット
- uspto-grants-1993_03
- 特許番号
- US05198208
反応ノート
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