Potassium hydroxy sulfite → 2-(4-(1H-1,2,4-triazol-1-yl)benzyl)-5-methyl-3-(methylsulfinyl)-7-neopentyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione

HRID 535894노트

반응식

HRID 535894 반응식
[N:1]1([C:6]2[CH:31]=[CH:30][C:9]([CH2:10][N:11]3[C:19]([S:20][CH3:21])=[C:18]4[C:13]([N:14]([CH2:25][C:26]([CH3:29])([CH3:28])[CH3:27])[C:15](=[O:24])[N:16]([CH3:23])[C:17]4=[O:22])=[N:12]3)=[CH:8][CH:7]=2)[CH:5]=[N:4][CH:3]=[N:2]1.[OH:32]OS([O-])=O.[K+]>C(Cl)Cl.CO>[N:1]1([C:6]2[CH:31]=[CH:30][C:9]([CH2:10][N:11]3[C:19]([S:20]([CH3:21])=[O:32])=[C:18]4[C:13]([N:14]([CH2:25][C:26]([CH3:28])([CH3:27])[CH3:29])[C:15](=[O:24])[N:16]([CH3:23])[C:17]4=[O:22])=[N:12]3)=[CH:8][CH:7]=2)[CH:5]=[N:4][CH:3]=[N:2]1

참가 물질

5

반응물 2

HCID 23707502Potassium hydroxy sulfiteHCID 462094022-(4-(1H-1,2,4-triazol-1-yl)benzyl)-5-methyl-3-(methylthio)-7-neopentyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione

생성물 1

HCID 462206432-(4-(1H-1,2,4-triazol-1-yl)benzyl)-5-methyl-3-(methylsulfinyl)-7-neopentyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione수율 48.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

실험 절차

2-(4-(1H-1,2,4-triazol-1-yl)benzyl)-5-methyl-3-(methylthio)-7-neopentyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (16 mg, 0.036 mmol) is dissolved in CH2Cl2 (500 μL) and MeOH (500 μL), and then an aqueous solution of Oxone (22.4 mg, 0.036 mmol) is added. The reaction mixture is stirred at room temperature for 2 days, and then purified by a semi-preparative HPLC to give 8 mg of product as off-white solids. MS (ESI) m/z 456.2 [M+H]+.

후처리

  1. custompurified by a semi-preparative HPLC

출처 및 근거

ORD 기록
ord-c2f0171a27c64a76aac9b425d594e055
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859564B2

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