Methyl iodide → HCID 5302363, 화합물

HRID 559042노트

반응식

HRID 559042 반응식
[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

참가 물질

9

반응물 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 1458133-NitropyrroleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 5302363HCID 5302363, 화합물수율 87.8%

시약·촉매·용매 4

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-9cf79b0d4fcd477cb1ddff31f12438c3
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063058B2

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