HRID1709869

反应详情

EQUATION

反应方程式

HRID 1709869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a magnetically stirred solution of ethyl isonicotinate in dry tetrahydrofuran at 0° C. and under an atmosphere of nitrogen is slowly added a solution 2.2 equivalents of 3,4-difluorophenyl magnesium bromide in tetrahydrofuran. The solution is stirred at ambient temperature of 4 hr and is poured into an icy solution of ammonium chloride. The mixture is extracted with methylene chloride, and the organic phase is dried (sodium sulfate). The solvent is removed in vacuo to give a solid. This solid is recrystallized from methylene chloride/hexane to give the title compound as a white, crystalline solid, mp 147°-149° C.

WORKUP

后处理

  1. extractionThe mixture is extracted with methylene chloride
  2. dry with materialthe organic phase is dried (sodium sulfate)
  3. customThe solvent is removed in vacuo
  4. customto give a solid
  5. customThis solid is recrystallized from methylene chloride/hexane