Phosphorus oxychloride → Ethyl 4,6-dichloropicolinate
反応式
[CH2:1]([O:3][C:4](=[O:13])[C:5]1[N+:6]([O-])=[CH:7][CH:8]=[C:9]([Cl:11])[CH:10]=1)[CH3:2].P(Cl)(Cl)([Cl:16])=O>>[CH2:1]([O:3][C:4](=[O:13])[C:5]1[CH:10]=[C:9]([Cl:11])[CH:8]=[C:7]([Cl:16])[N:6]=1)[CH3:2]参加物
3
反応条件
- 温度
- 0 °C
実験手順
4-Chloropicolinic acid ethyl ester N-oxide (1.6 g, 8 mmol) was added to 4 mL of phosphorus oxychloride at 0° C. and stirred at 0° C. for one hour. The solution was then heated at 100° C. for four hours. Excess POCl3 was removed in vacuo, and the residue was dissolved in ethyl acetate, washed with cold sodium bicarbonate solution, and extracted with ethyl acetate. Removal of the solvent gave 4,6-dichloropicolinic acid ethyl ester (compound A) as an off-white solid (1.12 g, 64%). The methyl ester can be made by an analogous procedure.
後処理
- temperatureThe solution was then heated at 100° C. for four hours
- customExcess POCl3 was removed in vacuo
- dissolutionthe residue was dissolved in ethyl acetate
- washwashed with cold sodium bicarbonate solution
- extractionextracted with ethyl acetate
- customRemoval of the solvent
出典と根拠
- ORDレコード
- ord-a55ce29bd4fc4f87b8dc4536635736cd
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08236795B2
反応ノート
読み込み中…