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Methyl iodide → HCID 136207705, 화합물

HRID 361615
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HRID 361615 반응식
[OH:1][N:2]=[CH:3][C:4]1[C:12]2[C:7](=[C:8]([CH3:14])[CH:9]=[CH:10][C:11]=2[CH3:13])[NH:6][C:5]=1[C:15]([O:17][CH3:18])=[O:16].CI.[C:21](=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:21][O:1][N:2]=[CH:3][C:4]1[C:12]2[C:7](=[C:8]([CH3:14])[CH:9]=[CH:10][C:11]=2[CH3:13])[NH:6][C:5]=1[C:15]([O:17][CH3:18])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 136365331HCID 136365331, 화합물

생성물 1

HCID 136207705HCID 136207705, 화합물수율 25%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 0.8 g (3.25 mmol) of methyl 3-(hydroxyiminomethyl)-4,7-dimethylindole-2-carboxylate, 0.60 g (4.23 mmol) of methyl iodide, 0.59 g (4.23 mmol) of potassium carbonate and 20 ml of acetonitrile was refluxed for 19 hours. After potassium carbonate was removed by filtration, acetonitrile was distilled off under reduced pressure. The residue was dissolved in ethyl acetate, washed with water three times and dried over anhydrous magnesium sulfate. The crude crystals were purified by silica gel column chromatography to provide 210 mg of light yellow crystals. Yield: 25%

후처리

  1. temperaturewas refluxed for 19 hours
  2. customAfter potassium carbonate was removed by filtration, acetonitrile
  3. distillationwas distilled off under reduced pressure
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with water three times
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe crude crystals were purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-6451de8f802942398b6ac7cb6ee539c8
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05866594

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