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

HRID 1024622노트

반응식

HRID 1024622 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-95a9db6860084cd4b9f8baa759799f62
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722691B2

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