反应详情

To a mixture of 2.2 g of 4-oxo-1,3-piperidinedicarboxylic acid 3-ethyl 1-[2-(trimethylsilyl)ethyl]ester and 1.2 g of valeramidine hydrochloride in 15 ml of dry ethyl alcohol is added 7 ml of 1M sodium methoxide in methanol. The resulting mixture is stirred and heated under reflux for 25 minutes. The reaction mixture is allowed to cool, filtered and the solid washed with ethyl alcohol. The combined filtrates are evaporated in vacuo without heat to give an oily solid. Ether and water are added to the residue followed by refrigeration. The resulting crystalline solid is collected, washed with ether and air dried to give 0.8 g of the desired product as a crystalline solid, m.p. 152°-155° C.

1. temperatureheated
2. temperatureunder reflux for 25 minutes
3. temperatureto cool
4. filtrationfiltered
5. washthe solid washed with ethyl alcohol
6. customThe combined filtrates are evaporated in vacuo
7. temperaturewithout heat
8. customto give an oily solid
9. customThe resulting crystalline solid is collected
10. washwashed with ether and air
11. customdried