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Water → {1-[1-(benzyloxy)-1H-pyrazol-5-yl]-2-ethylbutyl}amine

HRID 2243152
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HRID 2243152 반응식
[N:1]([CH:4]([C:10]1[N:14]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:13]=[CH:12][CH:11]=1)[CH:5]([CH2:8][CH3:9])[CH2:6][CH3:7])=[N+]=[N-].O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[CH2:16]([O:15][N:14]1[C:10]([CH:4]([NH2:1])[CH:5]([CH2:8][CH3:9])[CH2:6][CH3:7])=[CH:11][CH:12]=[N:13]1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 866000085-(1-Azido-2-ethylbutyl)-1-(benzyloxy)-1H-pyrazole

생성물 1

HCID 68595201{1-[1-(benzyloxy)-1H-pyrazol-5-yl]-2-ethylbutyl}amine수율 76.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

5-(1-Azido-2-ethylbutyl)-1-(benzyloxy)-1H-pyrazole (0.269 g, 0.90 mmol) was dissolved in THF (20 mL). Distilled water (0.40 mL, 22.5 mmol) was added, followed by triphenyl phosphine (0.590 g, 2.25 mmol). The mixture was refluxed for 2 h, cooled to ambient temperature and concentrated in vacuo. This produced a crude oil that was purified on a Biotage column (hexane/EtOAc, 1:1) to afford the product as a colorless oil (0.188 g, 76%). Mass Spectrum (+ESI): 274.2 (M+H)+.

후처리

  1. temperatureThe mixture was refluxed for 2 h
  2. concentrationconcentrated in vacuo
  3. customThis produced a crude oil that
  4. customwas purified on a Biotage column (hexane/EtOAc, 1:1)

출처 및 근거

ORD 기록
ord-625fd1fa685b4e19843a82b00606ea45
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07674813B2

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