تفاعل #10413

معادلة التفاعل

4,5-difluoroanthranilic acid

acetic acid

hypochlorous acid tert-butyl ester

→

3-chloro-4,5-difluoroanthranilic acid

المردود 100.8%

المذيبات

dichloromethane

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   غسيلwashed with water and brine
2. 2
   تجفيفThe organic layer is dried over MgSO4
3. 3
   ترشيحfiltered
4. 4
   تركيزconcentrated
5. 5
   أخرىThe resulting residue is purified via flash column chromatography (5% isopropyl alcohol/1% formic acid/94% dichloromethane)

الإجراء التجريبي

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+).

المصدر