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

HRID 859188ノート

反応式

HRID 859188 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 27583572-(2,2-difluoropropylamino)ethanol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

  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.)

出典と根拠

ORDレコード
ord-46faf2a20dca41949a90f15cffe2da3c
出典データセット
uspto-grants-2006_12
特許番号
US07151097B2

反応ノート

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