HRID49830

反应详情

EQUATION

反应方程式

HRID 49830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A solution of 4-fluorobenzonitrile (1.00 g, 8.26 mmol) and morpholine (0.77 mL, 9.08 mmol) in dimethyl sulfoxide (40 mL) was treated with 37% KF on alumina, and the mixture was heated at 150° C. for 5 h. After cooling, the mixture was diluted with EtOAc and filtered through diatomaceous earth. The filtrate was washed with water (3×), brine (1×), and then dried with magnesium sulfate. The extract was concentrated and the residue was purified by chromatography (SiO2, 20 to 30% EtOAc in hexanes) yielding 930 mg (60%) of the title compound.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationfiltered through diatomaceous earth
  3. washThe filtrate was washed with water (3×), brine (1×)
  4. dry with materialdried with magnesium sulfate
  5. concentrationThe extract was concentrated
  6. customthe residue was purified by chromatography (SiO2, 20 to 30% EtOAc in hexanes)