Methyl iodide → 4-Methyl-2-(methylsulfanyl)pyrimidine

HRID 42556

반응식

HRID 42556 반응식
[OH-].[Na+].Cl.[CH3:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([SH:11])[N:6]=1.I[CH3:13]>O>[CH3:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([S:11][CH3:13])[N:6]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 1784286872-Mercapto-4-methylpyrimidine hydrochloride

생성물 1

HCID 8212614-Methyl-2-(methylsulfanyl)pyrimidine수율 86.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of NaOH (7.46 g, 186.4 mmol) in water (120 mL), 4-methylpyrimidine-2-thiol hydrochloride (13.78 g, 84.7 mmol) was added and subsequently iodomethane (13.23 g, 93.2 mmol) was added dropwise under argon atmosphere. It was stirred at room temperature for 2 h. It was extracted with CH2Cl2 (×2). The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford 10.26 g of the desired compound (yield: 86%).

후처리

  1. extractionIt was extracted with CH2Cl2 (×2)
  2. dry with materialThe organic phase was dried over Na2SO4
  3. concentrationconcentrated to dryness
  4. customThe crude product obtained
  5. customwas purified by chromatography on silica gel
  6. temperatureof increasing polarity as eluent

출처 및 근거

ORD 기록
ord-28d9962299d84e278f896f2ad27afb03
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536194B2

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