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

HRID 1514406ノート

反応式

HRID 1514406 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-3d097722860d4ba3a29d4cf7f1820570
出典データセット
uspto-grants-2012_07
特許番号
US08222266B2

反応ノート

読み込み中…