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Water → n-({1-[2-(Benzofuran-3-yl)ethyl]-4-piperidyl}methyl)-n-methylamine

HRID 430603
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인쇄 미리보기

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HRID 430603 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[O:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9]([CH2:16][C:17]([N:19]2[CH2:24][CH2:23][CH:22]([C:25]([NH:27][CH3:28])=O)[CH2:21][CH2:20]2)=O)=[CH:8]1.O.[OH-].[Na+]>O1CCCC1>[O:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9]([CH2:16][CH2:17][N:19]2[CH2:20][CH2:21][CH:22]([CH2:25][NH:27][CH3:28])[CH2:23][CH2:24]2)=[CH:8]1
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참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 155123851-(Benzofuran-3-ylacetyl)-n-methyl-4-piperidinecarboxamideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 15512386n-({1-[2-(Benzofuran-3-yl)ethyl]-4-piperidyl}methyl)-n-methylamine

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

반응 조건

온도
60 °C

실험 절차

7.6 g of lithium aluminium hydride are added in portions to a solution of 28.7 g of the product obtained in Step C in 1.5 litres of tetrahydrofuran heated at 60°C. After 18 hours at reflux, the reaction mixture is hydrolysed by the addition of 5.24 ml of water, 4.2 ml of 20% sodium hydroxide solution and then 19.2 ml of water. After filtration, drying and concentration under reduced pressure, the expected product is isolated. The hydrochloride thereof recrystallises from methanol.

후처리

  1. temperatureAfter 18 hours at reflux
  2. filtrationAfter filtration
  3. customdrying
  4. concentrationconcentration under reduced pressure

출처 및 근거

ORD 기록
ord-fbfa6618b2eb4e50963005041e31c705
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06323217B2

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