Ethyl vinyl ether → Isobutyl (R)-(+)-2-(1-Ethoxyethoxy)propionate

HRID 2085616노트

반응식

HRID 2085616 반응식
[CH:1]([O:3][CH2:4][CH3:5])=[CH2:2].[C:6]([O:11][CH2:12][CH:13]([CH3:15])[CH3:14])(=[O:10])[C@@H:7]([CH3:9])[OH:8]>P(Cl)(Cl)(Cl)=O.C(OCC)(=O)C>[CH2:1]([O:3][CH:4]([O:8][C@H:7]([CH3:9])[C:6]([O:11][CH2:12][CH:13]([CH3:15])[CH3:14])=[O:10])[CH3:5])[CH3:2]

참가 물질

5

실험 절차

17.2 g of dehydrated ethyl vinyl ether was dropwise added to a mixture of 32.7 g of isobutyl (R)-(+)-lactate and 0.3 g of phosphorus oxychloride which was being stirred at room temperature, so that the internal temperature of the reaction system could be kept at 40° C. or less. Then, the resulting mixture was stirred at room temperature overnight. After the reaction, thereto was added 200 ml of ethyl acetate, followed by washing with a saturated aqueous sodium hydrogen carbonate solution, water and a saturated aqueous sodium chloride solution in this order. The washed material was dried over anhydrous sodium sulfate and then subjected to vacuum distillation to remove the solvent. The resulting concentrate was subjected to distillation to obtain 40.1 g (yield: 91.8%) of an oily title compound (diastereomixture).

후처리

  1. customcould be kept at 40° C. or less
  2. stirringThen, the resulting mixture was stirred at room temperature overnight
  3. customAfter the reaction
  4. washby washing with a saturated aqueous sodium hydrogen carbonate solution, water
  5. dry with materialThe washed material was dried over anhydrous sodium sulfate
  6. distillationsubjected to vacuum distillation
  7. customto remove the solvent
  8. concentrationThe resulting concentrate
  9. distillationwas subjected to distillation

출처 및 근거

ORD 기록
ord-58adff885dc94022a50f0cc7f5e2c31f
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06720463B1

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