Sodium sulfate decahydrate → 2-(4-Benzylpiperazin-1-yl)ethan-1-amine

HRID 1162342ノート

反応式

HRID 1162342 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:19][CH2:18][N:17]([CH2:20][C:21]#[N:22])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH2:7]([N:14]1[CH2:15][CH2:16][N:17]([CH2:20][CH2:21][NH2:22])[CH2:18][CH2:19]1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 38557212-(4-Benzylpiperazin-1-yl)acetonitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 27353312-(4-Benzylpiperazin-1-yl)ethan-1-amine収率 95%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a suspension of lithium aluminum hydride (5.0 g) in anhydrous THF (150 ml) was added a solution of (4-benzyl-1-piperazinyl)acetonitrile (11 g) obtained in Example 95a) in anhydrous THF (50 ml) under ice-cooling. The reaction solution was refluxed for 3 hours, to the reaction solution was then added sodium sulfate decahydrate (420 g) under ice-cooling, and mixed for 15 hours. The reaction solution was diluted with THF, the precipitate obtained by decantation was filtered off, and the solvent was distilled off under reduced pressure to obtain the title compound as pale yellow liquid (10 g, 95%).

後処理

  1. temperaturecooling
  2. temperatureThe reaction solution was refluxed for 3 hours, to the reaction solution
  3. additionmixed for 15 hours
  4. customthe precipitate obtained by decantation
  5. filtrationwas filtered off
  6. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-b8dd6ce48ac149cba9524242005e5ca5
出典データセット
uspto-grants-2010_10
特許番号
US07820673B2

反応ノート

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