反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([CH:11]([CH:19]([CH3:21])[CH3:20])[C:12]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[O:13])[N:4]=1.[H-].[Na+].[CH3:24][O:25][CH2:26]Cl>CN(C=O)C>[CH3:10][O:9][C:7]1[CH:8]=[C:3]([O:2][CH3:1])[N:4]=[C:5]([CH:11]([CH:19]([CH3:21])[CH3:20])[C:12]([N:14]([CH2:24][O:25][CH3:26])[S:15]([CH3:18])(=[O:17])=[O:16])=[O:13])[N:6]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
2.0 g of 2-(4,6-dimethoxypyrimidin-2-yl)-3-methyl-N-methylsulfonylbutyric acid amide was placed in a round bottomed flask, and was dissolved in 50 ml of DMF. To the resultant solution, was gradually added 0.28 g of 60% sodium hydride, and the mixture was stirred at room temperature for one hour. Thereafter, 1.0 g of chloromethyl methyl ether was added dropwise to the resultant mixture, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was then poured into ice water, and was extracted with 200 ml of diethyl ether, followed by drying with anhydrous sodium sulfate. After filtrating the inorganic salt, the solvent was distilled off under reduced pressure. An oily product thus obtained was purified by silica gel column chromatography (developing solvent: N-hexane/ethyl acetate=10/l ) to obtain 1.8 g of the aimed product of colorless transparent viscous liquid (yield=78.3%) having a refractive index (nD20) of 1.4976.
後処理
- stirringthe mixture was stirred at room temperature for 2 hours
- extractionwas extracted with 200 ml of diethyl ether
- dry with materialby drying with anhydrous sodium sulfate
- filtrationAfter filtrating the inorganic salt
- distillationthe solvent was distilled off under reduced pressure
- customAn oily product thus obtained
- customwas purified by silica gel column chromatography (developing solvent: N-hexane/ethyl acetate=10/l )
出典と根拠
- ORDレコード
- ord-ca31222bec234d1980fa24b5aabbc145
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05418212
関連ノート
読み込み中…