Ethylene Glycol → Ethyl 2-methyl-1,3-dioxolane-2-propionate

HRID 1627780

반응식

HRID 1627780 반응식
[C:1]([O:8][CH2:9][CH3:10])(=[O:7])[CH2:2][CH2:3][C:4]([CH3:6])=[O:5].[CH2:11](O)[CH2:12][OH:13].C1(C)C=CC(S(O)(=O)=O)=CC=1.[NH+]1C=CC=CC=1.O>C1(C)C=CC=CC=1>[CH3:6][C:4]1([CH2:3][CH2:2][C:1]([O:8][CH2:9][CH3:10])=[O:7])[O:13][CH2:12][CH2:11][O:5]1

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 962WaterHCID 10883Ethyl levulinateHCID 22033616Pyridinium.p-toluenesulfonate

생성물 1

HCID 70332Ethyl 2-methyl-1,3-dioxolane-2-propionate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

In a flask equipped by a Dean-Stark trap, a mixture of ethyl levulinate (28.83 g; 200 mmol), ethylene glycol (37.24 g; 600 mmol) and a catalytic amount of pyridinium para-toluenesulfonic acid in toluene (200 mL) was heated at reflux until the theoretical amount of water was distilled off. After cooling, the mixture was washed with a saturated solution of sodium hydrogenocarbonate. The basic layer was extracted with diethylether and the organics were combined, then washed with brine and water. The organic layer was dried over sodium sulphatesulphate and concentrated under reduced pressure to afford the ethyl 3-(2-methyl-1,3-dioxolan-2-yl)propanoate as a colorless oil.

후처리

  1. customIn a flask equipped by a Dean-Stark trap
  2. distillationwas distilled off
  3. temperatureAfter cooling
  4. washthe mixture was washed with a saturated solution of sodium hydrogenocarbonate
  5. extractionThe basic layer was extracted with diethylether
  6. washwashed with brine and water
  7. dry with materialThe organic layer was dried over sodium sulphatesulphate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ef41ac51bcf841e29afb641fc0b8899b
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785638B2

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