反応 #998442

反応方程式

4-cyanophenol

1-bromo-3,3-dimethylbutane

potassium carbonate

potassium iodide

→

desired intermediate

収率 89.0%

4-(3,3-Dimethylbutoxy)-benzonitrile

収率 89.0%

溶媒

acetone

acetone

反応条件

後処理

1. 1
   温度heat
2. 2
   温度at reflux for 48 h
3. 3
   ろ過filter
4. 4
   その他evaporate
5. 5
   その他Purify by chromatography on silica gel eluting with hexane/EtOAc (10 and 9:1)

実験手順

Mix 4-cyanophenol (1.2 g, 10 mmol), 1-bromo-3,3-dimethylbutane (5.3 g, 32 mmol), powdered potassium carbonate (4.14 g, 30 mmol), and powdered potassium iodide (166 mg, 1 mmol) in acetone (60 mL). Stir under inert atmosphere and heat at reflux for 48 h. Cool the reaction mixture to ambient temperature. Dilute with acetone, filter and evaporate. Purify by chromatography on silica gel eluting with hexane/EtOAc (10 and 9:1) to obtain the desired intermediate (1.8 g, 89%). MS (ES+) m/z: 221 (M+NH4)+.

出典