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Methanol → 4-(3-amino-1H-pyrazol-1-yl)butan-1-ol

HRID 546086
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HRID 546086 반응식
[N+:1]([C:4]1[CH:8]=[CH:7][N:6]([CH2:9][C:10]#[C:11][CH2:12][OH:13])[N:5]=1)([O-])=O.CO.NN>C(OCC)(=O)C.[Ni].O>[NH2:1][C:4]1[CH:8]=[CH:7][N:6]([CH2:9][CH2:10][CH2:11][CH2:12][OH:13])[N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 887MethanolHCID 9321HydrazineHCID 671932964-(3-Nitro-pyrazol-1-yl)-but-2-yn-1-ol

생성물 1

HCID 204512994-(3-amino-1H-pyrazol-1-yl)butan-1-ol수율 98%

시약·촉매·용매 3

HCID 935Nickel촉매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

The 4-(3-nitro-pyrazol-1-yl)-but-2-yn-1-ol (prepared in example 52, 113 mg, 0.62 mmol) was dissolved in ethyl acetate (3 mL) and methanol (3 mL) was added. While stirring, a 50% slurry of raney nickel in water (1.3 mL) was added followed by hydrazine (400 μL). Immediate effervescence was observed. The reaction continued to stir and bubble for 25 min. The reaction was passed through a plug of celite and concentrated in vacuo to afford 4-(3-amino-pyrazol-1-yl)-butan-1-ol (93 mg, 98%) as a clear oil: ESI-LRMS m/e calcd for C7H13N3O [M+] 155.11, found 156.32 [M+H+].

후처리

  1. stirringto stir
  2. custombubble for 25 min
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-8148d61361804ced87872c86395c433e
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07935699B2

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