反応 #302867

反応方程式

carbamate

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

methyl amine

CO2

→

2-aminonicotinic acid methyl amide

収率 97.0%

溶媒

dioxane

ethanol

反応条件

後処理

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

実験手順

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.).

出典