CID 86596527 → (3-(2-(4-bromophenyl)-1-(4-chlorophenyl)-6-oxo-1H-purin-9(6H)-yl)phenylsulfonyl)methyl acetate

HRID 1024622ノート

反応式

HRID 1024622 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]([C:30]3[CH:35]=[CH:34][C:33]([Cl:36])=[CH:32][CH:31]=3)[C:10](=[O:29])[C:11]3[N:12]=[CH:13][N:14]([C:17]4[CH:18]=[C:19]([S:23][CH2:24][O:25][C:26](=[O:28])[CH3:27])[CH:20]=[CH:21][CH:22]=4)[C:15]=3[N:16]=2)=[CH:4][CH:3]=1.C(O)(=O)C.[OH2:41].[OH2:42].O.O.O.O.C1(=O)OOOOC(=O)C2=CC=CC=C12.[Mg]>CO.ClCCl>[C:26]([O:25][CH2:24][S:23]([C:19]1[CH:20]=[CH:21][CH:22]=[C:17]([N:14]2[CH:13]=[N:12][C:11]3[C:10](=[O:29])[N:9]([C:30]4[CH:31]=[CH:32][C:33]([Cl:36])=[CH:34][CH:35]=4)[C:8]([C:5]4[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][CH:6]=4)=[N:16][C:15]2=3)[CH:18]=1)(=[O:42])=[O:41])(=[O:28])[CH3:27]

参加物

5

反応物 2

HCID 86596527CID 86596527HCID 131731396acetic acid (3-(2-(4-bromophenyl)-1-(4-chlorophenyl)-6-oxo-1H-purin-9(6H)-yl)phenylthio)methyl acetate

生成物 1

HCID 57899397(3-(2-(4-bromophenyl)-1-(4-chlorophenyl)-6-oxo-1H-purin-9(6H)-yl)phenylsulfonyl)methyl acetate

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of acetic acid (3-(2-(4-bromophenyl)-1-(4-chlorophenyl)-6-oxo-1H-purin-9(6H)-yl)phenylthio)methyl acetate (3, 2.1 g, 3.6 mmol) in methanol (12 mL), dichloromethane (36 mL), magnesium monoperoxy phthalate hexahydrate (1.9 g, 3.97 mmol) is added at 0° C. The resulting solution is stirred at rt for 12 h. The reaction is quenched with the addition of saturated solution of sodium bicarbonate, and extracted with dichloromethane. The organic layer is dried over Na2SO4, concentrated. The crude product is purified by column chromatography to afford (3-(2-(4-bromophenyl)-1-(4-chlorophenyl)-6-oxo-1H-purin-9(6H)-yl)phenylsulfonyl)methyl acetate (4).

後処理

  1. customThe reaction is quenched with the addition of saturated solution of sodium bicarbonate
  2. extractionextracted with dichloromethane
  3. dry with materialThe organic layer is dried over Na2SO4
  4. concentrationconcentrated
  5. customThe crude product is purified by column chromatography

出典と根拠

ORDレコード
ord-95a9db6860084cd4b9f8baa759799f62
出典データセット
uspto-grants-2014_05
特許番号
US08722691B2

反応ノート

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