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Methanol → 2-Methanesulfonyl-5-methyl-4-pyridin-3-yl-pyrimidine

HRID 1514408
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HRID 1514408 반응식
[CH3:1][C:2]1[C:3]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)=[N:4][C:5](SC)=[N:6][CH:7]=1.O[O:17][S:18]([O-:20])=O.[K+].[CH3:22]O>>[CH3:22][S:18]([C:5]1[N:4]=[C:3]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)[C:2]([CH3:1])=[CH:7][N:6]=1)(=[O:20])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 23707502Potassium hydroxy sulfiteHCID 59242786HCID 59242786, 화합물

생성물 1

HCID 686973182-Methanesulfonyl-5-methyl-4-pyridin-3-yl-pyrimidine수율 88%

실험 절차

A solution of 5-methyl-2-methylsulfanyl-4-pyridin-3-yl-pyrimidine (1.28 g, 5.90 mmol) in MeOH (45 ml) was cooled at 0° C. and then an aqueous solution of oxone (11 g, 17.95 mmol in 45 ml of water) was added dropwise. After 15 minutes, ice bath was removed and the stirring continue for 3 hours. The mixture was neutralized with solid NaHCO3 and the product was extracted with ethyl acetate. The organic phase was dried (Na2SO4) and evaporated to give 1.3 g of the title compound as a white powder (88% yield).

후처리

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
  • customice bath was removed
  • waitthe stirring continue for 3 hours
  • extractionthe product was extracted with ethyl acetate
  • dry with materialThe organic phase was dried (Na2SO4)
  • customevaporated
  • 출처 및 근거

    ORD 기록
    ord-f33826bba26143329662b10d8da64daa
    출처 데이터셋
    uspto-grants-2012_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08222266B2

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