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

HRID 1155065노트

반응식

HRID 1155065 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-6f2ce2ad1fe448d69a3bf21d73a91289
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04299834

반응 노트

불러오는 중…