反応 #10413

反応方程式

4,5-difluoroanthranilic acid

acetic acid

hypochlorous acid tert-butyl ester

→

3-chloro-4,5-difluoroanthranilic acid

収率 100.8%

溶媒

dichloromethane

ethyl acetate

反応条件

後処理

1. 1
   洗浄washed with water and brine
2. 2
   乾燥The organic layer is dried over MgSO4
3. 3
   ろ過filtered
4. 4
   濃縮concentrated
5. 5
   その他The resulting residue is purified via flash column chromatography (5% isopropyl alcohol/1% formic acid/94% dichloromethane)

実験手順

To a solution of 4,5-difluoroanthranilic acid (2.45 g, 14.2 mmol) in dichloromethane (25 mL) is added acetic acid (10 mL) and hypochlorous acid tert-butyl ester (1.75 mL, 15.6 mmol). After 2 hours, the reaction mixture is diluted with ethyl acetate and washed with water and brine. The organic layer is dried over MgSO4, filtered, and concentrated. The resulting residue is purified via flash column chromatography (5% isopropyl alcohol/1% formic acid/94% dichloromethane) to afford 3-chloro-4,5-difluoroanthranilic acid as an oil (2.97 g). MS CI: m/z 206 (M+).

出典