Aluminium lithium hydride → 2-(2,2-difluoropropylamino)ethanol

HRID 859188노트

반응식

HRID 859188 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[F:7][C:8]([F:16])([CH3:15])[C:9]([NH:11][CH2:12][CH2:13][OH:14])=O>C(OCC)C>[F:7][C:8]([F:16])([CH3:15])[CH2:9][NH:11][CH2:12][CH2:13][OH:14]

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 261889002,2-difluoro-N-(2-hydroxyethyl)propanamide

생성물 1

HCID 27583572-(2,2-difluoropropylamino)ethanol

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a stirred solution of lithium aluminum hydride (5.5 g, 146 mmol) in diethyl ether (85 ml) was added a solution of 2,2-difluoro-N-(2-hydroxy-ethyl)-propionamide (11.2 g, 73 mmol) in diethyl ether (55 ml) dropwise at such a rate to maintain a gentle reflux. After an additional 1.5 hours, the reaction was quenched with sodium sulfate decahydrate, diluted with ethyl acetate and allowed to stir for 18 hours. The mixture was filtered with the aid of diatomaceous earth, washing with ethyl acetate. The filtrate was concentrated in vacuo and fractionally distilled (11 torr, collecting fractions distilling at 75–88° C.) to afford the title compound (I-3c) as a colorless oil, 4.5 g.

후처리

  1. temperatureto maintain a gentle reflux
  2. customthe reaction was quenched with sodium sulfate decahydrate
  3. additiondiluted with ethyl acetate
  4. filtrationThe mixture was filtered with the aid of diatomaceous earth
  5. washwashing with ethyl acetate
  6. concentrationThe filtrate was concentrated in vacuo
  7. distillationfractionally distilled
  8. distillation(11 torr, collecting fractions distilling at 75–88° C.)

출처 및 근거

ORD 기록
ord-46faf2a20dca41949a90f15cffe2da3c
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07151097B2

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