反応式
CS([C:5]1[N:10]=[C:9]([C:11]2[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:13][CH:12]=2)[CH:8]=[C:7]([C:21]([F:24])([F:23])[F:22])[N:6]=1)(=O)=O.[NH2:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=1>CC#N>[CH3:20][S:17]([C:14]1[CH:15]=[CH:16][C:11]([C:9]2[CH:8]=[C:7]([C:21]([F:24])([F:23])[F:22])[N:6]=[C:5]([NH:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=3)[N:10]=2)=[CH:12][CH:13]=1)(=[O:19])=[O:18]参加物
4
実験手順
To a stirred solution of 2-(methylsulfonyl)-4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidine (0.10 g, 0.26 mmol) in MeCN (4 ml) was added 2-(aminomethyl)-pyridine (0.14, 5 eq) and the resultant solution heated under reflux for 3 h. The cooled reaction mixture was concentrated in vacuo and purified by SPE chromatography using chloroform, diethyl ether, ethyl acetate, acetone and methanol as the eluotropic series of solvents. Concentration in vacuo of the combined fractions containing pure product gave the title compound as a colourless solid (0.086 g, 80%).
後処理
- temperatureunder reflux for 3 h
- customThe cooled reaction mixture
- concentrationwas concentrated in vacuo
- custompurified by SPE chromatography
- concentrationConcentration in vacuo of the combined fractions
- additioncontaining pure product
出典と根拠
- ORDレコード
- ord-aef2424bcef946ada83aa023afe11928
- 出典データセット
- uspto-grants-2004_08
- 特許番号
- US06780870B2
関連ノート
読み込み中…