反応式
[CH2:1]([Li])[CH3:2].[Cl:4][C:5]1[CH:6]=[C:7]([CH:24]=[CH:25][CH:26]=1)[C:8]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH2:17][CH2:18][N:19]([CH2:22][CH3:23])[CH2:20][CH3:21])=[CH:12][CH:11]=1)=[O:9].[Cl-].[NH4+]>CCOCC>[Cl:4][C:5]1[CH:6]=[C:7]([CH:24]=[CH:25][CH:26]=1)[C:8]([CH2:1][CH3:2])([OH:9])[C:10]1[CH:11]=[CH:12][C:13]([O:16][CH2:17][CH2:18][N:19]([CH2:20][CH3:21])[CH2:22][CH3:23])=[CH:14][CH:15]=1参加物
5
実験手順
To 125 ml. of a 0.8 molar ethereal ethyl lithium solution a solution of 13.3 g. of 3-chloro-4'-[2-(diethylamino)-ethoxy]-benzophenone in 160 ml. of ether is added dropwise, with stirring under argon atmosphere, at a temperature between -20° C. and -15° C. The reaction mixture is then stirred at room temperature for one hour, and is decomposed with a saturated aqueous ammonium chloride solution, under cooling. The aqueous phase is extracted with ether, the ethereal phases are combined and washed to neutral with water. After drying over anhydrous magnesium sulfate, ether is distilled off under reduced pressure. Crystallization of the solid residue from n-hexane yields 8.9 g. of the title compound, melting at 64° to 65° C.
後処理
- stirringThe reaction mixture is then stirred at room temperature for one hour
- temperatureunder cooling
- extractionThe aqueous phase is extracted with ether
- washwashed to neutral with water
- dry with materialAfter drying over anhydrous magnesium sulfate, ether
- distillationis distilled off under reduced pressure
- customCrystallization of the solid residue from n-hexane
- customyields 8.9 g
出典と根拠
- ORDレコード
- ord-fc4d06e26eda4476b08a3f37189dff98
- 出典データセット
- uspto-grants-1986_08
- 特許番号
- US04605672
関連ノート
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