반응 #58502

반응 방정식

6-(1-methylpiperidin-4-ylcarbonyl)-pyridine

HCl ethanol

→

6-(1-methylpiperidin-4-ylcarbonyl)-pyridine 2HCl

수율 63.0%

용매

ethanol

반응 조건

후처리

1. 1
   기타remove the solvent
2. 2
   온도heat
3. 3
   온도under reflux for 30 minutes
4. 4
   세척filtered-off the precipitate, rinse with 20 ml isopropanol
5. 5
   기타dry under vacuum at 50° C.

실험 절차

Resuspend the crude 2-amino-(6-(1-methylpiperidin-4-ylcarbonyl)-pyridine (14.5 g, 66.2 mmol) in ethanol (30 mL), add 2.5M HCl/ethanol (100 mL), stir the mixture for 30 minutes, and then remove the solvent under reduce pressure. Resuspend the resulting solid in 125 ml isopropanol and heat under reflux for 30 minutes. Cool the reaction mixture to room temperature, filtered-off the precipitate, rinse with 20 ml isopropanol, and dry under vacuum at 50° C. to obtain 2-amino-(6-(1-methylpiperidin-4-ylcarbonyl)-pyridine 2HCl (11 g, 63% yield corrected by HPLC % w/w).

출처