HRID1282481

反应详情

EQUATION

反应方程式

HRID 1282481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Into a reactor were introduced 1.38 g (10.0 mmol) of 4-chlorobenzonitrile, 1.68 g (20.0 mmol) of 2-methyl-3 butyne-2-ol, 2.7 mg (0.015 mmol) of palladium, 1.4 mg (0.0075 mmol) of copper iodide, 17.6 mg (0.045 mmol) of the 1,1-diphenyl-2-(dicyclohexylphosphine)propene obtained in Example 2, 4.0 mL (0.055 mmol) of diisopropylamine, and 4.0 ml of N,N-dimethylformamide under a nitrogen atmosphere. The resultant reaction mixture was stirred at 100° C. for 23 hours and then cooled. Thereafter, the solvent was removed under pressure. The concentrate was purified by column clromatography to obtain 1.56 g (84%) of 4-(4-cyanophenyl)-2-methyl-3-butyne-2-ol as white crystals.

WORKUP

后处理

  1. customThe resultant reaction mixture
  2. temperaturecooled
  3. customThereafter, the solvent was removed under pressure
  4. customThe concentrate was purified by column clromatography