Phosphorus oxychloride → 4-Chloro-5-methyl-2-(methylsulfanyl)pyrimidine

HRID 1514406

반응식

HRID 1514406 반응식
[CH3:1][C:2]1[C:3](=O)[NH:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1.O=P(Cl)(Cl)[Cl:13]>O1CCOCC1>[Cl:13][C:3]1[C:2]([CH3:1])=[CH:7][N:6]=[C:5]([S:8][CH3:9])[N:4]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 2405755-Methyl-2-(methylthio)pyrimidin-4(3H)-one

생성물 1

HCID 235627084-Chloro-5-methyl-2-(methylsulfanyl)pyrimidine수율 89%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 5-methyl-2-methylsulfanyl-3H-pyrimidin-4-one (6.86 g, 44 mmol) and POCl3 (14 ml) in dioxane (60 ml) was refluxed for 2 hours. The solvent was removed under vacuum and the residue was quenched with ice and extracted with diethylether. The organic phase was dried (Na2SO4) and evaporated to give 6.8 g of the title compound as oil that was used in the next step without further purification. (89% yield)

후처리

  1. temperaturewas refluxed for 2 hours
  2. customThe solvent was removed under vacuum
  3. customthe residue was quenched with ice
  4. extractionextracted with diethylether
  5. dry with materialThe organic phase was dried (Na2SO4)
  6. customevaporated

출처 및 근거

ORD 기록
ord-3d097722860d4ba3a29d4cf7f1820570
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08222266B2

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