HRID1744568

反应详情

EQUATION

反应方程式

HRID 1744568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-(4-Fluorophenyl)-3-methylpyrazole-4-carboxylic acid (1.0 g), 5-amino-2-n-hexyloxybenzonitrile (1.0 g), triethylamine (1.4 g) and diethyl cyanophosphate (1.2 g) were added to dimethylformamide (20 ml) and the mixture was stirred at room temperature for 1 h. The reaction mixture was added into water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. n-Hexane was added to the residue to allow crystallization. The crystals were recrystallized from ethyl acetate to give the title compound (0.5 g), melting point: 160–161° C.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customafter which the solvent was evaporated under reduced pressure
  5. additionn-Hexane was added to the residue
  6. customcrystallization
  7. customThe crystals were recrystallized from ethyl acetate