HRID354733

反应详情

EQUATION

反应方程式

HRID 354733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a stirred mixture of isopropyl bromide (246.0 g; 2.0 mol), triethylamine (160.0 g; 4.0 mol), and solid sodium hydroxide pels (160.0 g; 4.0 mol) is added 4-methoxyphenylacetonitrile (147.18 g, 95% pure=139.85 g; 0.95 mol) over a 30-minute period at 60° C. Following this addition the reaction mixture is stirred at 68°-74° C. for 6 hours. The reaction mixture is then cooled to 45° C. and water (205 ml) is added. The mixture is subsequently stirred for 15 minutes with cooling. The organic and aqueous phases are then separated and the excess isopropyl bromide and triethylamine is distilled from the organic phase. This method gives 189.7 g of product which is 92.6% pure. This corresponds to an effective yield of 98.7%.

WORKUP

后处理

  1. additionthis addition the reaction mixture
  2. stirringThe mixture is subsequently stirred for 15 minutes
  3. temperaturewith cooling
  4. customThe organic and aqueous phases are then separated
  5. distillationthe excess isopropyl bromide and triethylamine is distilled from the organic phase