반응 #1568067

반응 방정식

5-Bromo-2-nitrophenol

methyl 2-chloro-2,2-difluoroacetate

Potassium carbonate

→

title compound

수율 30.5%

2-(Difluoromethoxy)-4-bromo-1-nitrobenzene

수율 30.5%

용매

DMF

ethyl acetate

반응 조건

후처리

1. 1
   온도The reaction was cooled to room temperature
2. 2
   세척The organic solution was washed with water (20 mL), brine (20 mL)
3. 3
   건조dried over sodium sulphate
4. 4
   농축concentrated in vacuo
5. 5
   기타The residue was purified by silica gel column chromatography
6. 6
   세척eluting with 20% dichloromethane in hexanes

실험 절차

5-Bromo-2-nitrophenol (1 g, 4.59 mmol) and methyl 2-chloro-2,2-difluoroacetate (991 mg, 6.9 mmol) were dissolved in dry DMF (3 mL). Potassium carbonate (1.27 g, 9.18 mmol) was added and the reaction was stirred at 120° C. for 1 hour. The reaction was cooled to room temperature and diluted with ethyl acetate (20 mL). The organic solution was washed with water (20 mL), brine (20 mL), dried over sodium sulphate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with 20% dichloromethane in hexanes to afford the title compound as a dark brown oil (375 mg, 30%).

출처