Reacción #302867

Ecuación de reacción

carbamate

1H-Pyrido[2,3-d]oxazin-2,4-dione

methyl amine

CO2

→

2-aminonicotinic acid methyl amide

Rendimiento 97.0%

Disolventes

dioxane

ethanol

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaAfter cooling down to room temperature
2. 2
   Otrothe formed precipitate is removed by filtration
3. 3
   Concentraciónthe filtrate is concentrated to dryness

Procedimiento

14.96 g (0.09 mol) of 1H-Pyrido[2,3-d]oxazin-2,4-dione was suspended in 138 ml dioxane. The mixture is heated to 40° C. and 17 ml of a 33% solution of methyl amine in ethanol is added dropwise directly into the reaction mixture, to avoid carbamate formation with the evolving CO2. The reaction is allowed to continue for 90 minutes. After cooling down to room temperature, the formed precipitate is removed by filtration and the filtrate is concentrated to dryness. 13.2 g (97%) of 2-aminonicotinic acid methyl amide was isolated (m.p. 140-2° C.).

Fuente