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Ethylacetate methanol → {2-Ethyl-1-[1-(4-fluorobenzyl)-1H-1,2,4-triazol-5-yl]butyl}amine

HRID 2243137
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HRID 2243137 반응식
[N:1]([CH:4]([C:10]1[N:14]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=2)[N:13]=[CH:12][N:11]=1)[CH:5]([CH2:8][CH3:9])[CH2:6][CH3:7])=[N+]=[N-].CO.CCOC(C)=O>CCOC(C)=O.[Pd]>[CH2:8]([CH:5]([CH2:6][CH3:7])[CH:4]([NH2:1])[C:10]1[N:14]([CH2:15][C:16]2[CH:17]=[CH:18][C:19]([F:22])=[CH:20][CH:21]=2)[N:13]=[CH:12][N:11]=1)[CH3:9]
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참가 물질

5

반응물 2

HCID 21584119Ethylacetate methanolHCID 866000065-(1-Azido-2-ethylbutyl)-1-(4-fluorobenzyl)-1H-1,2,4-triazole

생성물 1

HCID 68593905{2-Ethyl-1-[1-(4-fluorobenzyl)-1H-1,2,4-triazol-5-yl]butyl}amine수율 68%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매2회

실험 절차

To a suspension of 5% Pd/C in EtOAc was added a solution of 5-(1-azido-2-ethylbutyl)-1-(4-fluorobenzyl)-1H-1,2,4-triazole in EtOAc and the mixture was shaken on a Parr apparatus for 2 h under 3 atm of H2. The mixture was filtered through Celite, washed several times with EtOAc, concentrated in vacuo, and purified by column chromatography (SiO2, EtOAc, then, MeOH/EtOAc, 1:9, then 1:4) to yield 68% of the amine.

후처리

  1. filtrationThe mixture was filtered through Celite
  2. washwashed several times with EtOAc
  3. concentrationconcentrated in vacuo
  4. custompurified by column chromatography (SiO2, EtOAc

출처 및 근거

ORD 기록
ord-6b06fe6e7916438a8d0c2a49c154b0b1
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07674813B2

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