HRID322568

反应详情

EQUATION

反应方程式

HRID 322568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

A mixture of 2-[2-(4-fluorophenyl)ethyl]benzonitrile (8.03 g, 35.6 mmol, 1 equiv) and aq. NaOH (10N; 16 mL, 160 mmol, 4.5 equiv) in ethylene glycol (100 mL) was heated to 190° C. for 69 h. After allowing the reaction mixture to cool, H2O (300 mL) was added, followed by 12N HCl (16 mL). This mixture was extracted with CHCl3 (1×100 mL) and the organic layer was then washed with H2O (2×50 mL). The organic layer was dried (anh. Na2SO4) and rotary evaporated (90° C.). This provided 7.44 g (85.4%) of a light-yellow solid.

WORKUP

后处理

  1. temperatureto cool
  2. extractionThis mixture was extracted with CHCl3 (1×100 mL)
  3. washthe organic layer was then washed with H2O (2×50 mL)
  4. dry with materialThe organic layer was dried (anh. Na2SO4)
  5. customrotary evaporated (90° C.)