Methylhydrazine → 1-Methyl-3-phenyl-1H-pyrazol-5-amine

HRID 402477

반응식

HRID 402477 반응식
[C:1]([CH2:9][C:10]#[N:11])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:12][NH:13][NH2:14]>CO>[CH3:12][N:13]1[C:10]([NH2:11])=[CH:9][C:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[N:14]1

참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 64799Benzoylacetonitrile

생성물 1

HCID 5177791-Methyl-3-phenyl-1H-pyrazol-5-amine수율 71.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of benzoyl acetonitrile (2.0 g, 13.778 mmol) and methyl hydrazine (0.698, 15.156 mmol) in methanol (10 mL) was irradiated under microwave conditions at 110° C. for 90 min. The reaction mixture was cooled to rt and poured into rapidly stirred ice cold water. The obtained solid was collected by filtration, dried under vacuum and triturated with a mixture of pentane-hexane (˜10 mL) to yield a white solid (1.7 g, 71%). [1H-NMR (CDCl3, 300 MHz) δ 7.82-7.65 (m, 2H), 7.45-7.20 (m, 3H), 5.90 (s, 1H), 3.75 (s, 3H), 3.55 (s, 2H); LCMS RtA=0.824 min; [M+H]+=174.1]

후처리

  1. customwas irradiated under microwave conditions at 110° C. for 90 min
  2. additionpoured into rapidly stirred ice cold water
  3. filtrationThe obtained solid was collected by filtration
  4. customdried under vacuum
  5. customtriturated with a mixture of pentane-hexane (˜10 mL)

출처 및 근거

ORD 기록
ord-13a444bbc6634ce09bcbd8cf08acef13
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08742106B2

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