Water → 1-methyl-4-nitro-1H-pyrazole

HRID 84801

반응식

HRID 84801 반응식
[N+:1]([C:4]1[CH:5]=[N:6][NH:7][CH:8]=1)([O-:3])=[O:2].I[CH3:10].[H-].[Na+].O>CN(C=O)C.CCOC(C)=O>[CH3:10][N:6]1[CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:8]=[N:7]1

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 163764-nitro-1H-pyrazoleHCID 24758Sodium hydride

생성물 1

HCID 198951-methyl-4-nitro-1H-pyrazole수율 87.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-nitro-1H-pyrazole (1.13 g, 10.0 mmol) and iodomethane (1.25 mL, 20.0 mmol) in DMF (12 mL), NaH (60% in mineral oil, 0.600 g, 15.0 mmol) was added. The mixture was stirred for 18 h. Water and EtOAc were added. The organic phase was separated, washed with water, dried over Na2SO4, concentrated in vacuo to give 1-methyl-4-nitro-1H-pyrazole as a solid (1.11 g).

후처리

  1. customThe organic phase was separated
  2. washwashed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-70caa30616674d57aacfc9d4bd670837
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846928B2

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