반응 #88209

반응 방정식

water

4-bromo-2,6-difluoroaniline

AcOH

H2O

AcOH

H2O

→

desired product

5-Bromo-1,3-difluoro-2-nitro-benzene

반응 조건

후처리

1. 1
   추출extracted with Et2O
2. 2
   기타obtained from another reaction
3. 3
   농축The mixture was concentrated
4. 4
   기타A precipitate was formed
5. 5
   기타separated by filtration
6. 6
   농축The filtrate was concentrated

실험 절차

A solution of 4-bromo-2,6-difluoroaniline (240 mmol) in AcOH (150 mL) was added dropwise to a suspension of NaBO3.4 H2O (325 mmol) in AcOH (450 mL) at 70° C. during 30 min. Another 2080 mmol of NaBO3.4 H2O were added over 5 h to the mixture. During this period the mixture was stirred at 70° C. The mixture was poured into water and extracted with Et2O. The organic layer was combined with another Et2O solution obtained from another reaction using the same conditions described above. The mixture was concentrated. A precipitate was formed and separated by filtration. The filtrate was concentrated to afford the desired product after flash column chromatography (SiO2, petroleum ether).

출처