Hydrochloric Acid → 2-Amino-4,4-difluorobutanoic acid hydrochloride

HRID 19323노트

반응식

HRID 19323 반응식
C([O:3][C:4](=[O:19])[C:5]([NH:15]C(=O)C)([CH2:11][CH:12]([F:14])[F:13])C(OCC)=O)C.[ClH:20]>>[ClH:20].[NH2:15][CH:5]([CH2:11][CH:12]([F:14])[F:13])[C:4]([OH:19])=[O:3]

참가 물질

3

반응물 2

HCID 313Hydrochloric AcidHCID 17749984Diethyl 2-acetamido-2-(2,2-difluoroethyl)malonate

생성물 1

HCID 470033322-Amino-4,4-difluorobutanoic acid hydrochloride수율 97%

실험 절차

In a flask was placed 2-acetylamino-2-(2,2-difluoro-ethyl)-malonic acid diethyl ester (8.94 g, 31.78 mmol) and 6N aqueous hydrochloric acid (140 mL). This mixture was refluxed overnight. After this time, the mixture was cooled to room temperature and extracted with diethyl ether (100 mL) the aqueous layer was concentrated in vacuo, azeotroped with acetonitrile and dried under high vacuum to afford 2-amino-4,4-difluoro-butyric acid hydrochloride salt (5.39 g, 97%) as a cream colored solid.

후처리

  1. customIn a flask was placed
  2. temperatureThis mixture was refluxed overnight
  3. extractionextracted with diethyl ether (100 mL) the aqueous layer
  4. concentrationwas concentrated in vacuo
  5. customazeotroped with acetonitrile
  6. customdried under high vacuum

출처 및 근거

ORD 기록
ord-c9fda19b50b74a45a68557364533658c
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741327B2

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