Methyl iodide → HCID 5302363、化合物

HRID 559042ノート

反応式

HRID 559042 の反応式
[H-].[Na+].[N+:3]([C:6]1[CH:10]=[CH:9][NH:8][CH:7]=1)([O-:5])=[O:4].I[CH3:12].[H][H]>CCCCCC.CN(C=O)C.CCOC(C)=O.O>[CH3:12][N:8]1[CH:9]=[CH:10][C:6]([N+:3]([O-:5])=[O:4])=[CH:7]1

参加物

9

反応物 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 1458133-NitropyrroleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 5302363HCID 5302363、化合物収率 87.8%

試薬・触媒・溶媒 4

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To sodium hydride (300 mg, 60% in mineral oil, 7.50 mmol) in a flask, which was washed with hexane twice, a solution of 3-nitropyrrole (500 mg, 4.46 mmol) and iodomethane (0.560 mL, 8.97 mmol) in DMF (4 mL) was added. Hydrogen gas evolved. The mixture was then stirred at room temperature for 20 h. Water and EtOAc were added. Organic phase was separated, washed with water, dried over Na2SO4, concentrated in vacuo to give 1-methyl-3-nitro-1H-pyrrole (494 mg).

後処理

  1. customOrganic 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-9cf79b0d4fcd477cb1ddff31f12438c3
出典データセット
uspto-grants-2011_11
特許番号
US08063058B2

反応ノート

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