Water → 1-methyl-4-nitro-1H-pyrazole

HRID 84801

反応式

HRID 84801 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 198951-methyl-4-nitro-1H-pyrazole収率 87.3%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-70caa30616674d57aacfc9d4bd670837
出典データセット
uspto-grants-2014_09
特許番号
US08846928B2

関連ノート

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