Water → N-Benzylputrescine

HRID 1493887노트

반응식

HRID 1493887 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 152999N-Benzylputrescine수율 57.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d583353b775646039a92d8465ca5e4ec
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05025033

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