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Ammonium Chloride → 4-amino-3-methyl-1H-Pyrazole-1-acetonitrile

HRID 577744
노트
인쇄 미리보기

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HRID 577744 반응식
[CH3:1][C:2]1[C:6]([N+:7]([O-])=O)=[CH:5][N:4]([CH2:10][C:11]#[N:12])[N:3]=1.[NH4+].[Cl-]>CO.O.[Fe]>[NH2:7][C:6]1[C:2]([CH3:1])=[N:3][N:4]([CH2:10][C:11]#[N:12])[CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 19620685(3-Methyl-4-nitro-1H-pyrazol-1-YL)acetonitrile

생성물 1

HCID 866796734-amino-3-methyl-1H-Pyrazole-1-acetonitrile수율 20.6%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 887Methanol용매HCID 962Water용매

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온도
80 °C

실험 절차

A mixture of (3-methyl-4-nitro-1H-pyrazol-1-yl)acetonitrile (2.6 g, 15.7 mmol), NH4Cl (3.4 g, 62.7 mmol) and Fe powder (3.5 g, 62.7 mmol) in MeOH (60 mL) and water (12 mL) was stirred at 80° C. for 2 days. The mixture was filtered, concentrated and the residue was purified by flash chromatography (MeOH: CH2Cl2 20:1) to give the title compound (440 mg, 15% yield) as brown oil.

후처리

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. customthe residue was purified by flash chromatography (MeOH: CH2Cl2 20:1)

출처 및 근거

ORD 기록
ord-616e9d627a014a508b830f9e3eac7751
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040547B2

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