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Methyl iodide → 4,6-Dichloro-1-methyl-1H-pyrrolo[3,2-c]pyridine

HRID 1022427
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HRID 1022427 반응식
[Cl:1][C:2]1[C:7]2[CH:8]=[CH:9][NH:10][C:6]=2[CH:5]=[C:4]([Cl:11])[N:3]=1.[H-].[Na+].I[CH3:15]>O1CCCC1>[Cl:1][C:2]1[C:7]2[CH:8]=[CH:9][N:10]([CH3:15])[C:6]=2[CH:5]=[C:4]([Cl:11])[N:3]=1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 53589884,6-Dichloro-1H-pyrrolo[3,2-c]pyridine

생성물 1

HCID 140553384,6-Dichloro-1-methyl-1H-pyrrolo[3,2-c]pyridine수율 96%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

A solution of 4,6-dichloro-1H-pyrrolo[3,2-c]pyridine (270 mg, 1.44 mmol) in tetrahydrofuran (4 mL) at 0° C. was treated with a 60% dispersion of sodium hydride in mineral oil (69.3 mg, 2.89 mmol) followed by iodomethane (225 mg, 1.59 mmol). After stirring at 0° C. for 0.5 h, the reaction mixture was allowed to warm to room temperature and was stirred at room temperature for 5 h. At this time, the resulting mixture was quenched with a saturated aqueous sodium bicarbonate solution. The reaction mixture was extracted with ethyl acetate. The combined organics were washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and concentrated in vacuo. Flash chromatography (30% ethyl acetate/hexanes) afforded 4,6-dichloro-1-methyl-1H-pyrrolo[3,2-c]pyridine (278 mg, 95.8%). LC-MS calcd. for C8H6Cl2N2 [(M+H)+] 201, obsd. 200.8.

후처리

  1. temperatureto warm to room temperature
  2. stirringwas stirred at room temperature for 5 h
  3. customAt this time, the resulting mixture was quenched with a saturated aqueous sodium bicarbonate solution
  4. extractionThe reaction mixture was extracted with ethyl acetate
  5. washThe combined organics were washed with a saturated aqueous sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b6b9ce3b0306406d9845b643d2b95d14
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722661B2

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