HRID1194079

反应详情

EQUATION

反应方程式

HRID 1194079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 6-methyl-2-pyridineethanol (97.2 g), p-fluorobenzonitrile (85.8 g) and dry tetrahydrofuran (600 ml) was added 60% sodium hydride in oil (29.0 g) in small portions with ice-cooling and stirring and the mixture was further stirred for 2 hours. The reaction mixture was poured in ice-water and extracted with ethyl ether. The ethyl ether layer was washed with water, dried (MgSO4) and concentrated, and the residue was crystallized from hexane to give 4-[2-(6-methyl-2-pyridyl)ethoxy]benzonitrile. Yield: 85.9 g (50.1%); m.p.: 66°-67° C.

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture was further stirred for 2 hours
  3. extractionextracted with ethyl ether
  4. washThe ethyl ether layer was washed with water
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customthe residue was crystallized from hexane