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 535894ノート

反応式

HRID 535894 の反応式
[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

参加物

5

反応物 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

生成物 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)-dione収率 48.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

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]+.

後処理

  1. custompurified by a semi-preparative HPLC

出典と根拠

ORDレコード
ord-c2f0171a27c64a76aac9b425d594e055
出典データセット
uspto-grants-2014_10
特許番号
US08859564B2

反応ノート

読み込み中…