反応式
[H-].[Na+:2].C(O[C:6]([C:8]1[CH:9]=[N:10][N:11]([CH3:22])[C:12]=1[NH:13][C:14]1[CH:19]=[CH:18][C:17](C)=[CH:16][C:15]=1[NH2:21])=[O:7])C.[CH3:23][S:24]([CH3:26])=[O:25]>>[CH3:23][S:24]([CH2-:26])=[O:25].[Na+:2].[CH3:22][N:11]1[C:12]2[NH:13][C:14]3[CH:19]=[C:18]([CH3:23])[CH:17]=[CH:16][C:15]=3[NH:21][C:6](=[O:7])[C:8]=2[CH:9]=[N:10]1参加物
5
反応条件
- 温度
- 65 °C
実験手順
Sodium (methylsulphinyl)methanide (22.7 mmol) was prepared from sodium hydride (60% dispersion in oil, 912 mg, 22.7 mmol) and anhydrous dimethyl sulphoxide (5.5 ml) by heating at 65° C. until a solution was observed. To this was added a solution of 5-(2-amino-4-methyl-phenylamino)-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester from Example E2.2 (3.56 g, 13.0 mmol) in anhydrous dimethyl sulphoxide (10 ml), and stirring continued at 65° C. for 30 min. The mixture was then poured into ice (200 ml), the resulting solid collected and purified by flash chromatography on silica gel (eluant; 10% methanol:90% dichloromethane) to yield the title compound (1.12 g, 38%).
後処理
- customthe resulting solid collected
- custompurified by flash chromatography on silica gel (eluant; 10% methanol:90% dichloromethane)
出典と根拠
- ORDレコード
- ord-1a2ea833a6924951bd3f9c75e6a1db45
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08202858B2
関連ノート
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