HRID2035527
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwere added
- temperatureheated
- temperatureat reflux for 8 hours
- temperatureAfter cooling
- customthe solvent was evaporated
- addition10 mL of water was added to the residue
- additionby adding 2 mol/L hydrochloric acid in water under ice cooling
- extractionextracted with chloroform
- dry with materialthe extract was dried on anhydrous sodium sulfate
- customThe solvent was evaporated
- customthe residue was recrystallized from chloroform-hexane