反応 #60308

反応方程式

3-Chloro-2,4-difluoro-benzoic acid

H2SO4

nitric acid

→

clean desired product

収率 95.0%

3-Chloro-2,4-difluoro-5-nitro-benzoic acid

収率 95.0%

反応条件

後処理

1. 1
   workup.ADDITIONThe yellow slurry is poured onto ice water (100 mL)
2. 2
   抽出The aqueous mixture is extracted with diethyl ether (3×)
3. 3
   乾燥The organic extracts are dried (Na2SO4)
4. 4
   濃縮concentrated under reduced pressure

実験手順

3-Chloro-2,4-difluoro-benzoic acid 1a (3.00 g, 15.6 mmol) is added to a stirred solution of concentrated H2SO4 (16 mL) and fuming nitric acid (0.85 mL, 20.3 mmol). After 3 hours a precipitate forms. The yellow slurry is poured onto ice water (100 mL). The aqueous mixture is extracted with diethyl ether (3×). The organic extracts are dried (Na2SO4) and concentrated under reduced pressure to give 3.50 g (95%) of clean desired product as a pale yellow solid.

出典