1,3-Dibromopropane → 1,3-Bis(4-fluoro-2-iodophenoxy)propane
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([I:9])[CH:3]=1.Br[CH2:11][CH2:12][CH2:13]Br.[C:15](=[O:18])([O-])[O-].[K+].[K+]>CC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:11][CH2:12][CH2:13][O:18][C:15]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][C:4]=2[I:9])=[C:4]([I:9])[CH:3]=1参加物
5
実験手順
To a solution of 15.00 g (63.03 mmol) of 4-fluoro-2-iodophenol (P7), Preparation 7 and 6.40 g (31.68 mmol) of 1,3-dibromopropane in 200 mL of acetone add 26.00 g (188.4 mmol) of potassium carbonate. Reflux the resulting reaction mixture for 24 hours. Cool the reaction mixture to room temperature, filter it, and concentrate the filtrate by rotary evaporation. Crystallize the resulting solid from acetonitrile to yield 12.00 g (74%) of (P8) as a white crystalline solid.
後処理
- temperatureReflux
- customthe resulting reaction mixture for 24 hours
- filtrationfilter it
- concentrationconcentrate the filtrate
- customby rotary evaporation
- customCrystallize the resulting solid from acetonitrile
- customto yield 12.00 g (74%) of (P8) as a white crystalline solid
出典と根拠
- ORDレコード
- ord-d97b5df56a5a4d84ba81625083555a2a
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09029487B2
反応ノート
読み込み中…