Water → N-Benzylputrescine

HRID 1493887ノート

反応式

HRID 1493887 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([CH2:9][CH2:10][CH2:11][NH:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)#[N:8].O.[OH-].[Na+]>O1CCCC1>[CH2:13]([NH:12][CH2:11][CH2:10][CH2:9][CH2:7][NH2:8])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 30145704-(Benzylamino)butanenitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 152999N-Benzylputrescine収率 57.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a suspension of 1.1 g of lithium aluminum hydride in 50 ml of tetrahydrofuran was added slowly 2.9 g of N-(3-cyanopropyl)benzylamine (obtained in Reference Example 4) at room temperature. The reaction mixture was heated gently under reflux for 15 minutes and then allowed to cool. To the mixture was added dropwise and carefully 2.2 ml of water and then 1.8 ml of 10% aqueous sodium hydroxide. The resultant precipitate was filtered off, the filtrate was dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to give 1.7 g of N-benzyl-1,4-butanediamine as a colorless oil.

後処理

  1. temperatureThe reaction mixture was heated gently
  2. temperatureunder reflux for 15 minutes
  3. temperatureto cool
  4. additionTo the mixture was added dropwise
  5. filtrationThe resultant precipitate was filtered off
  6. dry with materialthe filtrate was dried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-d583353b775646039a92d8465ca5e4ec
出典データセット
uspto-grants-1991_06
特許番号
US05025033

反応ノート

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