Methyl iodide → 1-Methyl-5-nitro-1H-indole-3-carbaldehyde

HRID 618105

반응식

HRID 618105 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[NH:9][CH:8]=[C:7]2[CH:13]=[O:14])([O-:3])=[O:2].[C:15](=O)([O-])[O-].[K+].[K+].CI>CN(C)C=O>[CH3:15][N:9]1[C:10]2[C:6](=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:12][CH:11]=2)[C:7]([CH:13]=[O:14])=[CH:8]1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 2460395-nitro-1H-indole-3-carbaldehyde

생성물 1

HCID 128715121-Methyl-5-nitro-1H-indole-3-carbaldehyde수율 92.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

5-Nitroindole-3-carboxaldehyde (2 g) was dissolved in N,N-dimethylformamide (40 ml), and potassium carbonate (4.0 g) and methyl iodide (5 ml) were added thereto, followed by stirring at 60° C. for 24 hours. The reaction solution was subjected to partitioning with chloroform, methanol and water, and the organic layer was dried over magnesium sulfate. After concentration under reduced pressure, the residue was rinsed with ethyl acetate to give 1-methyl-5-nitroindole-3-carboxaldehyde (Compound III-2, 1.99 g).

후처리

  1. customto partitioning with chloroform, methanol and water
  2. dry with materialthe organic layer was dried over magnesium sulfate
  3. concentrationAfter concentration under reduced pressure
  4. washthe residue was rinsed with ethyl acetate

출처 및 근거

ORD 기록
ord-9b7c0d8c56f747a5a79040795b1e06b1
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952355

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