反応式
[H-].[Na+].[CH3:3][S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)(=[O:6])=[O:5].[CH:13]1([CH:18]([NH:20][C:21]2[CH:30]=[CH:29][CH:28]=[CH:27][C:22]=2C(OC)=O)[CH3:19])[CH2:17][CH2:16][CH2:15][CH2:14]1.Cl.[O:32]1CCC[CH2:33]1>COCCOC>[CH:13]1([CH:18]([NH:20][C:21]2[CH:22]=[CH:27][C:28]([C:33](=[O:32])[CH2:3][S:4]([C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=3)(=[O:6])=[O:5])=[CH:29][CH:30]=2)[CH3:19])[CH2:14][CH2:15][CH2:16][CH2:17]1参加物
実験手順
A solution of 864 mg. of sodium hydride and 5.3 g. of methylphenylsulfone in 20 ml. of 1,2-dimethoxyethane is stirred at 6° C. for one hour under an atmosphere of argon. To this solution is added a solution of 5.0 g. of methyl (1-cyclopentylethylamino)benzoate in 50 ml. of tetrahydrofuran and the reaction mixture is stirred at 60° C. for 1.5 hours. The mixture is cooled, poured onto ice, acidified with dilute hydrochloric acid and pH 3 and then extracted with chloroform. The organic layer is separated, washed with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate and then concentrated to dryness. The crude solid is chromatographed on silica gel, eluting with methylene chloride to yield 4'-(1cyclopentylethylamino)-2-(phenylsulfonyl)acetophenone.
後処理
- additionTo this solution is added a solution of 5.0 g
- temperatureThe mixture is cooled
- additionpoured onto ice
- extractionextracted with chloroform
- customThe organic layer is separated
- washwashed with water and saturated sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated to dryness
- customThe crude solid is chromatographed on silica gel
- washeluting with methylene chloride
出典と根拠
- ORDレコード
- ord-5d91c82e3b2d43059a90c136a85010c3
- 出典データセット
- uspto-grants-1981_03
- 特許番号
- US04259352
関連ノート
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