Methanol → Methyl 4-amino-6-chloro-5-fluoropicolinate
反応式
[NH2:1][C:2]1[C:7]([F:8])=[C:6]([Cl:9])[N:5]=[C:4]([C:10]([OH:12])=[O:11])[CH:3]=1.S(Cl)(Cl)=O.[CH3:17]O>O>[NH2:1][C:2]1[C:7]([F:8])=[C:6]([Cl:9])[N:5]=[C:4]([C:10]([O:12][CH3:17])=[O:11])[CH:3]=1参加物
5
反応条件
- 温度
- 50 °C
実験手順
To a solution of 4-amino-6-chloro-5-fluoropicolinic acid (23.8 g, 125 mmol) in MeOH (400 ml), cooled in an ice water bath, thionyl chloride (11.78 ml, 162 mmol) was added. The reaction mixture was heated to an internal temperature of 50° C., for 8 hours. The reaction mixture was then diluted with H2O, and extracted with EtOAC (3×100 mL). The combined organics were washed with Sat. NaCl, dried over Mg Sulfate, filtered and concentrated under vacuum to give methyl 4-amino-6-chloro-5-fluoropicolinate (21.9 g, 107 mmol, 86% yield).
後処理
- extractionextracted with EtOAC (3×100 mL)
- washThe combined organics were washed with Sat. NaCl
- dry with materialdried over Mg Sulfate
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-900fdc93d6034433a65e442fc56cdd91
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08754229B2
反応ノート
読み込み中…