反应详情

2,2-Dimethylpropyl 4-(4-cyanopyridin-2-yl)piperazine-1-carboxylate (143 mg) obtained in Example 2 was dissolved in ethanol (5 mL), and hydrazine acetate (140 mg) and potassium carbonate (328 mg) were added thereto and heated under reflux for 5 hours, then the reaction liquid was evaporated. Acetic anhydride (3 mL) was added to the resulting residue, and heated under reflux for 2 hours, then the reaction liquid was diluted with ethyl acetate, washed with water and saturated saline water, and dried with anhydrous sodium sulfate. The solvent was evaporated away, and the resulting residue was isolated and purified through thin-layer silica gel chromatography (chloroform/methanol=9/1) to obtain 7.6 mg of the entitled compound as a colorless oil.

1. temperatureheated
2. temperatureunder reflux for 5 hours
3. customthe reaction liquid
4. customwas evaporated
5. additionAcetic anhydride (3 mL) was added to the resulting residue
6. temperatureheated
7. temperatureunder reflux for 2 hours
8. customthe reaction liquid
9. washwashed with water and saturated saline water
10. dry with materialdried with anhydrous sodium sulfate
11. customThe solvent was evaporated away
12. customthe resulting residue was isolated
13. custompurified through thin-layer silica gel chromatography (chloroform/methanol=9/1)