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Methyl iodide → 5-Bromo-1,4-dimethyl-1,2-dihydropyridin-2-one

HRID 58052
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인쇄 미리보기

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HRID 58052 반응식
[Br:1][C:2]1[C:3]([CH3:9])=[CH:4][C:5](=[O:8])[NH:6][CH:7]=1.IC.[C:12](=O)([O-])[O-].[K+].[K+]>CS(C)=O>[Br:1][C:2]1[C:3]([CH3:9])=[CH:4][C:5](=[O:8])[N:6]([CH3:12])[CH:7]=1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 8199375-Bromo-2-hydroxy-4-methylpyridine

생성물 1

HCID 672818265-Bromo-1,4-dimethyl-1,2-dihydropyridin-2-one

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
60 °C

실험 절차

To a solution of 5-bromo-4-methylpyridin-2(1H)-one (164 mg, 0.872 mmol) and iodomethane (124 mg, 0.872 mmol) in DMSO (3 mL) was added potassium carbonate (121 mg, 0.872 mmol). The mixture was stirred at 60° C. overnight, filtered, and purified via preparative HPLC, eluting with a gradient of 20-70% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA) to give the title compound.

후처리

  1. filtrationfiltered
  2. custompurified via preparative HPLC
  3. washeluting with a gradient of 20-70% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA)

출처 및 근거

ORD 기록
ord-fe8fd08f64a148a9b12e5008fd63ca04
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09434743B2

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