Sodium Sulfate → 3-(Benzylamino)butan-1-ol

HRID 515442

反応式

HRID 515442 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].C([O:9][C:10](=O)[CH2:11][CH:12]([NH:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[CH3:13])C.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1(OC)CCCC1>[CH2:15]([NH:14][CH:12]([CH3:13])[CH2:11][CH2:10][OH:9])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

5

反応物 3

HCID 24436Sodium SulfateHCID 236384Ethyl 3-(benzylamino)butanoateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 104649043-(Benzylamino)butan-1-ol収率 87.4%

試薬・触媒・溶媒 1

HCID 138539Cyclopentyl methyl ether溶媒2 回

実験手順

To a suspension of lithium aluminum hydride (0.76 g, 20 mmol) in cyclopentylmethylether (20 mL) was added a solution of 3-benzylamino-butyric acid ethyl ester (2.10 g, 9.5 mmol) in cyclopentylmethylether (10 mL) dropwise at 0° C. under nitrogen atmosphere. The resulting mixture was warmed to room temperature and stirred for 3 hours. Then small amount of sodium sulfate saturated aqueous solution was added dropwise to quench the reaction at 0° C. and stirred for one hour. The resulting solid material was removed by filtration and the organic solution was concentrated to yield 3-benzylamino-butan-1-ol (1.49 g, 8.3 mmol, 87%) as colorless oil. The oil was used in the subsequent step without further purification.

後処理

  1. customto quench
  2. customthe reaction at 0° C.
  3. stirringstirred for one hour
  4. customThe resulting solid material was removed by filtration
  5. concentrationthe organic solution was concentrated

出典と根拠

ORDレコード
ord-b64286a5459f4c40a482100335b37efc
出典データセット
uspto-grants-2015_08
特許番号
US09108957B2

関連ノート

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