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

HRID 1155066ノート

反応式

HRID 1155066 の反応式
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

参加物

3

反応物 1

HCID 54364326HCID 54364326、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-aa39ce56751f4fe78d3eb3cbb3ba7fa0
出典データセット
uspto-grants-1981_11
特許番号
US04299834

反応ノート

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