Sodium ethoxide → 1,6-Naphthyridin-2(1H)-one, 5,8-dimethyl-
反応式
[NH2:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([CH3:9])[C:3]=1/[CH:10]=[CH:11]/[C:12]([O:14]CC)=O.C([O-])C.[Na+]>C(O)C>[CH3:9][C:4]1[N:5]=[CH:6][C:7]([CH3:8])=[C:2]2[C:3]=1[CH:10]=[CH:11][C:12](=[O:14])[NH:1]2参加物
4
反応条件
- 温度
- 80 °C
実験手順
A mixture of (E)-ethyl 3-(4-amino-2,5-dimethylpyridin-3-yl)acrylate (5 g, 22.7 mmol) and sodium ethanolate (6.2 g, 91 mmol) in ethanol (100 mL) was heated to 80° C. for 2 h. The reaction mixture was concentrated and diluted with water (50 mL). The aqueous phase was extracted with EtOAc (100 mL×3), and the combined organic layers were washed with saturated sodium chloride solution, dried with sodium sulfate, and concentrated to give 2.3 g of the product as a yellow solid. MS (ESI): m/z 175.1 [M+H]+.
後処理
- concentrationThe reaction mixture was concentrated
- additiondiluted with water (50 mL)
- extractionThe aqueous phase was extracted with EtOAc (100 mL×3)
- washthe combined organic layers were washed with saturated sodium chloride solution
- dry with materialdried with sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-9a749d6ff6294f38877a5ad4a12e0ff9
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08969349B2
反応ノート
読み込み中…