反応式
[CH:1]([Mg]Cl)=[CH2:2].[CH2:5]([C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[CH:14]=[O:15])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cl-].[NH4+].Cl>O1CCCC1>[CH2:5]([C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[CH:14]([OH:15])[CH:1]=[CH2:2])[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1参加物
実験手順
30 ml of a 1.6 molar solution of vinyl-magnesium chloride in tetrahydrofuran are introduced into 100 ml of absolute tetrahydrofuran at 0° C. 9.8 g (0.05 mole) of 2-benzylbenzaldehyde in 100 ml of absolute tetrahydrofuran are added dropwise whilst stirring and excluding moisture. The reaction mixture is stirred for 3 hours at 25° C. and is then cautiously decomposed by adding a cold saturated ammonium chloride solution and a few milliliters of 10% strength hydrochloric acid until the precipitate dissolves. The mixture is then extracted by shaking three times with ether and the combined ether phases are washed with sodium bisulfite solution, sodium bicarbonate solution and water, dried over sodium sulfate and concentrated under reduced pressure. 9.4 g of a yellowish oil, which is sufficiently pure for the further reactions, are obtained; nD21 =1.5855.
後処理
- stirringThe reaction mixture is stirred for 3 hours at 25° C.
- dissolutiondissolves
- extractionThe mixture is then extracted
- stirringby shaking three times with ether
- washthe combined ether phases are washed with sodium bisulfite solution, sodium bicarbonate solution and water
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customare obtained
出典と根拠
- ORDレコード
- ord-6e0aa55930224ed08f546ba417ad8acc
- 出典データセット
- uspto-grants-1982_08
- 特許番号
- US04344961
関連ノート
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