反应详情

温度

85 °C

Load 2-bromo-6-(1-methylpiperidin-4-ylcarbonyl)-piperidine (20 g, 70.67 mmol, 1 eq) in 73.6 ml of 7M NH3/ethylene glycol (530 mmol, 7.5 eq) into a 130 ml pressure autoclave, and add Cu2O (101 mg, 0.706 mmol, 0.01 eq) as a catalyst. Seal the autoclave and heat the reaction mixture to 85° C. at about 50 psi (345 kPa) for 20 hrs. Cool the reaction mixture to room temperature, transfer the organic layer to a 250 ml flask, and place the flask under reduce pressure to remove ammonia. Add water (70 mL) and of 30% NaOH (38 mL) and then extract the mixture with methyl t-butyl ether (MTBE)(5×100 ml). Combine the organic fractions and then dry with MgSO4, filter, and concentrate under reduce pressure to obtain crude 2-amino-(6-(1-methylpiperidin-4-ylcarbonyl)-pyridine (18.5 g).

1. customSeal the autoclave
2. temperatureCool the reaction mixture to room temperature
3. customto remove ammonia
4. extractionAdd water (70 mL) and of 30% NaOH (38 mL) and then extract the mixture with methyl t-butyl ether (MTBE)(5×100 ml)
5. dry with materialCombine the organic fractions and then dry with MgSO4
6. filtrationfilter
7. concentrationconcentrate