反应 #302867

反应方程式

carbamate

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

methyl amine

CO2

→

2-aminonicotinic acid methyl amide

收率 97.0%

溶剂

dioxane

ethanol

反应条件

后处理

1. 1
   温度After cooling down to room temperature
2. 2
   其他the formed precipitate is removed by filtration
3. 3
   浓缩the filtrate is concentrated to dryness

实验过程

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.).

来源