Phosphorus oxychloride → Dimethyl 4-chloropyridine-3,5-dicarboxylate
反応式
O=[C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][NH:5][CH:4]=[C:3]1[C:12]([O:14][CH3:15])=[O:13].O=P(Cl)(Cl)[Cl:18]>>[Cl:18][C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][N:5]=[CH:4][C:3]=1[C:12]([O:14][CH3:15])=[O:13]参加物
3
反応条件
- 温度
- 140 °C
実験手順
A mixture of dimethyl 4-oxo-1,4-dihydropyridine-3,5-dicarboxylate (3 g, crude) and POCl3 (10 mL) was heated to 140° C. in the sealed tube for 15 hours. The mixture was cooled to RT, poured into ice and extracted with ether. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated to afford the title compound as solid (yield 33.7%).
後処理
- temperatureThe mixture was cooled to RT
- additionpoured into ice
- extractionextracted with ether
- washThe organic layer was washed with brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-d14a058bf7e8446199a5ef4d0ec86e68
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440968B2
反応ノート
読み込み中…