HRID2041147

反应详情

EQUATION

反应方程式

HRID 2041147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

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 (1.0 and 9:1) to obtain the desired intermediate (1.8 g, 89%). MS (ES+) m/z: 221 (M+NH4)+.

WORKUP

后处理

  1. temperatureheat
  2. temperatureat reflux for 48 h
  3. filtrationfilter
  4. customevaporate
  5. customPurify by chromatography on silica gel eluting with hexane/EtOAc (1.0 and 9:1)