Reacción #554310

Ecuación de reacción

3-ethynylbenzaldehyde

ethyl alcohol

ethyl 3-aminocrotonate

allyl acetoacetate

→

desired compound

5-Ethoxycarbonyl-3-allyloxycarbonyl-1,4-dihydro-2,6-dimethyl-4-(3-ethynylphenyl)pyridine

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrothe reaction
2. 2
   Concentraciónthe reaction mixture was concentrated
3. 3
   Otroto give precipitate
4. 4
   LavadoAfter washing the obtained precipitate with ether
5. 5
   Otrothe precipitate was recrystallized from the mixture solution of n-pentane and diethyl ether (n-pentane : diethyl ether=3 : 1 by volume)

Procedimiento

In 20 ml of ethyl alcohol was dissolved 1.95 g (15 mmol) of 3-ethynylbenzaldehyde. Thereto were added 1.95 g (15 mmol) of ethyl 3-aminocrotonate and 2.1 g (15 mmol) of allyl acetoacetate, and the admixture was stirred with heating for 16 hours at 80° C. After completing the reaction, the reaction mixture was concentrated to give precipitate. After washing the obtained precipitate with ether, the precipitate was recrystallized from the mixture solution of n-pentane and diethyl ether (n-pentane : diethyl ether=3 : 1 by volume) to give 3.4 g of the desired compound of light yellow needle crystal (yield: 61.5%).

Fuente