Carbamate → 2-Amino-N-methylpyridine-3-carboxamide
反応式
[NH:1]1[C:6]2C=N[O:9][CH2:10][C:5]=2[C:4](=O)[CH2:3][C:2]1=O.C[NH2:14].[C:15](=O)([O-])[NH2:16].C(=O)=O>O1CCOCC1.C(O)C>[CH3:15][NH:16][C:10](=[O:9])[C:5]1[CH:4]=[CH:3][CH:2]=[N:1][C:6]=1[NH2:14]参加物
7
反応条件
- 温度
- 40 °C
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.).
後処理
- temperatureAfter cooling down to room temperature
- customthe formed precipitate is removed by filtration
- concentrationthe filtrate is concentrated to dryness
出典と根拠
- ORDレコード
- ord-b2fff7c590ea4b8b851c57434f503c61
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08192918B2
反応ノート
読み込み中…