반응 #60239

반응 방정식

HCl

Ammonium hydroxide

2,3,4-trifluoro-5-nitro-benzoic acid

2,3,4-Trifluoro-5-nitro-benzoic acid

ammonium hydroxide

→

pure desired product

수율 95.0%

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

수율 95.0%

용매

water

water

반응 조건

후처리

1. 1
   workup.STIRRINGwith stirring
2. 2
   온도the reaction mixture is cooled to 0° C.
3. 3
   추출extracted with diethyl ether (3×50 mL)
4. 4
   건조The combined organic extracts are dried (MgSO4)
5. 5
   농축concentrated under reduced pressure

실험 절차

Ammonium hydroxide solution (˜30% in water) (35 mL, 271 mmol) is added to a solution of 2,3,4-trifluoro-5-nitro-benzoic acid 2 (15 g, 67.8 mmol) in 30 mL water at 0° C. with stirring. Upon completion of ammonium hydroxide addition the reaction mixture is warmed to room temperature with stirring. After 2.5 hours, the reaction mixture is cooled to 0° C. and concentrated HCl is carefully added until pH of reaction mixture is near 0. The reaction mixture is diluted with water (30 mL) and extracted with diethyl ether (3×50 mL). The combined organic extracts are dried (MgSO4) and concentrated under reduced pressure to give 14 g (95%) of pure desired product: MS APCI (−) m/z 217 (M−1) detected.

출처