HRID2035527

反应详情

EQUATION

反应方程式

HRID 2035527 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

200 mg of 4,6-dichloropyridine-3-carboxyamide synthesized according to the method described in US2006/0217417 was dissolved in 2 mL of ethanol, to which 156 mg of cyclohexylamine and 203 mg of N,N-diisopropylethylamine were added, and heated at reflux for 8 hours. After cooling, the solvent was evaporated, and 10 mL of water was added to the residue, neutralized by adding 2 mol/L hydrochloric acid in water under ice cooling, extracted with chloroform, and the extract was dried on anhydrous sodium sulfate. The solvent was evaporated, and the residue was recrystallized from chloroform-hexane to obtain 243 mg (92%) of the title compound as colorless needle crystals.

WORKUP

后处理

  1. additionwere added
  2. temperatureheated
  3. temperatureat reflux for 8 hours
  4. temperatureAfter cooling
  5. customthe solvent was evaporated
  6. addition10 mL of water was added to the residue
  7. additionby adding 2 mol/L hydrochloric acid in water under ice cooling
  8. extractionextracted with chloroform
  9. dry with materialthe extract was dried on anhydrous sodium sulfate
  10. customThe solvent was evaporated
  11. customthe residue was recrystallized from chloroform-hexane