HCID 54364326, 화합물 → 1H-Purine, 8-(4-methoxy-2-(2-(methylthio)ethoxy)phenyl)-

HRID 1155066노트

반응식

HRID 1155066 반응식
COC1C=CC(C([NH:9][C:10]2[C:15]([NH:16][C:17](=O)[C:18]3[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][C:19]=3[O:26][CH2:27][CH2:28][S:29][CH3:30])=[CH:14][N:13]=[CH:12][N:11]=2)=O)=C(OCCSC)C=1>P(Cl)(Cl)(Cl)=O>[CH3:25][O:24][C:21]1[CH:22]=[CH:23][C:18]([C:17]2[NH:16][C:15]3[C:10](=[N:11][CH:12]=[N:13][CH:14]=3)[N:9]=2)=[C:19]([O:26][CH2:27][CH2:28][S:29][CH3:30])[CH:20]=1

참가 물질

3

반응물 1

HCID 54364326HCID 54364326, 화합물

생성물 1

HCID 30599141H-Purine, 8-(4-methoxy-2-(2-(methylthio)ethoxy)phenyl)-

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

An amount of 3.1 g of 4,5-bis-[4-methoxy-2-(2-methylmercapto-ethoxy)-benzoylamino]pyrimidine was refluxed in 25 ml of phosphorus oxychloride for two hours. After the phosphorus oxychloride was distilled off, the residue was taken up in water and filtered, and the product was precipitated by addition of sodium bicarbonate and recrystallized from ethanol. A further fraction was obtained by purification of the mother liquors over silicagel (eluate: methylene chloride/ethanol in a volume ratio of 19:1).

후처리

  1. distillationAfter the phosphorus oxychloride was distilled off
  2. filtrationfiltered
  3. customthe product was precipitated by addition of sodium bicarbonate
  4. customrecrystallized from ethanol
  5. customA further fraction was obtained by purification of the mother liquors over silicagel (eluate: methylene chloride/ethanol in a volume ratio of 19:1)

출처 및 근거

ORD 기록
ord-aa39ce56751f4fe78d3eb3cbb3ba7fa0
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04299834

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