Phosphorus oxychloride → 1H-Purine, 8-(2-methoxy-4-(methylthio)phenyl)-

HRID 1155065ノート

反応式

HRID 1155065 の反応式
Cl.Cl.[NH2:3][C:4]1[C:9]([NH2:10])=[CH:8][N:7]=[CH:6][N:5]=1.[CH3:11][O:12][C:13]1[CH:21]=[C:20]([S:22][CH3:23])[CH:19]=[CH:18][C:14]=1[C:15](Cl)=O.P(Cl)(Cl)(Cl)=O>C(O)C>[CH3:11][O:12][C:13]1[CH:21]=[C:20]([S:22][CH3:23])[CH:19]=[CH:18][C:14]=1[C:15]1[NH:10][C:9]2[C:4](=[N:5][CH:6]=[N:7][CH:8]=2)[N:3]=1

参加物

5

反応物 3

HCID 24813Phosphorus oxychlorideHCID 27595912-Methoxy-4-(methylthio)benzoyl chlorideHCID 20562693Pyrimidine-4,5-diamine dihydrochloride

生成物 1

HCID 30599131H-Purine, 8-(2-methoxy-4-(methylthio)phenyl)-

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4.1 g of 4,5-diamino-pyrimidine dihydrochloride, 7.1 g of 2-methoxy-4-methylmercapto-benzoylchloride, and 50 ml of phosphorus oxychloride was refluxed for three hours. The reaction mixture was evaporated until one-half of the original volume remained, and then the remaining mixture was poured into water. The precipitate that formed was dissolved in boiling ethanol, precipitated by addition of ether, and purified by chromatography on silicagel (eluate: methylene chloride/ethanol in a volume ratio of 19:1).

後処理

  1. temperaturewas refluxed for three hours
  2. customThe reaction mixture was evaporated until one-half of the original volume
  3. additionthe remaining mixture was poured into water
  4. customThe precipitate that formed
  5. dissolutionwas dissolved
  6. customprecipitated by addition of ether
  7. custompurified by chromatography on silicagel (eluate: methylene chloride/ethanol in a volume ratio of 19:1)

出典と根拠

ORDレコード
ord-6f2ce2ad1fe448d69a3bf21d73a91289
出典データセット
uspto-grants-1981_11
特許番号
US04299834

反応ノート

読み込み中…