反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21][C:20](Br)=[CH:19][CH:18]=2)([C:13]([F:16])([F:15])[F:14])[C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=1.C([Li])CCC.C(=O)=O.CC(C)=O.Cl[Si:37]([CH3:40])([CH3:39])[CH3:38]>O1CCCC1.CCCCCC>[CH3:38][Si:37]([CH3:40])([CH3:39])[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21][C:20]([Si:37]([CH3:40])([CH3:39])[CH3:38])=[CH:19][CH:18]=2)([C:13]([F:16])([F:15])[F:14])[C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=1参加物
反応条件
- 温度
- -78 °C
実験手順
To a solution of 4.62g (0.1 mole) 2,2-bis(4-bromophenyl)hexafluoropropane in 75 ml of anhydrous tetrahydrofuran was added dropwise 28 ml (0.4 moles) of a 1.4 molar solution of n-butyllithium in hexane while the reaction mixture was cooled in a dry ice-acetone slush. The reaction mixture was stirred for one half hour at -78° C. A dropwise addition of chlorotrimethylsilane (5 ml, 0.04 moles) was then made to the reaction mixture at -78° C. The stirring slurry was allowed to come to ambient temperature over 16 hours. To the reaction mixture was added 100 ml hexane. The organic layer was washed with 2×150 ml saturated sodium chloride solution and 2×150 ml water. The organic layer was dried, filtered, and concentrated to yield the white crystalline product 2,2-bis(4-trimethylsilylphenyl)hexafluoropropane.
後処理
- customwas then made to the reaction mixture at -78° C
- washThe organic layer was washed with 2×150 ml saturated sodium chloride solution and 2×150 ml water
- customThe organic layer was dried
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-7fd16d840cb54ef1b286bde73c439315
- 出典データセット
- uspto-grants-1987_03
- 特許番号
- US04649207
関連ノート
読み込み中…