Ethanol → Ethyl 2-(2-methylpyridin-3-yl)acetate

HRID 1526077

반응식

HRID 1526077 반응식
[CH3:1][C:2]1[C:7]([CH2:8][C:9]#N)=[CH:6][CH:5]=[CH:4][N:3]=1.S(=O)(=O)(O)O.C(=O)(O)[O-:17].[Na+].[CH2:21]([OH:23])[CH3:22]>>[CH2:21]([O:23][C:9](=[O:17])[CH2:8][C:7]1[C:2]([CH3:1])=[N:3][CH:4]=[CH:5][CH:6]=1)[CH3:22]

참가 물질

5

반응물 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 516892Sodium Bicarbonate2회HCID 190992862-(2-Methylpyridin-3-yl)acetonitrile

생성물 1

HCID 15169545Ethyl 2-(2-methylpyridin-3-yl)acetate

실험 절차

790 mg (5.98 mmol) of the compound from Example 38A are initially introduced into 10 ml ethanol, 4 ml concentrated sulfuric acid are added slowly and the mixture is heated under reflux for 6 h. After cooling, the mixture is neutralized with 6.00 g sodium bicarbonate and saturated sodium bicarbonate solution. The aqueous phase is extracted several times with ethyl acetate and the combined organic phases are dried over sodium sulfate, filtered and concentrated. The residue is reacted without further purification.

후처리

  1. additionare added slowly
  2. temperaturethe mixture is heated
  3. temperatureunder reflux for 6 h
  4. temperatureAfter cooling
  5. extractionThe aqueous phase is extracted several times with ethyl acetate
  6. dry with materialthe combined organic phases are dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue is reacted without further purification

출처 및 근거

ORD 기록
ord-26c686c181134a499eb02e8399b224bf
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09085572B2

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