반응 #1563944

반응 방정식

2-Chloro-2,2,-difluoroacetic acid sodium salt

Water

3-bromo-5-fluorophenol

K2CO3

→

desired compound

1-Bromo-3-(difluoromethoxy)-5-fluorobenzene

용매

ethyl acetate

DMF

반응 조건

후처리

1. 1
   workup.STIRRINGstirring
2. 2
   workup.WAITwas continued at 100° C. for 3 h
3. 3
   온도The reaction mixture was cooled to 25° C.
4. 4
   세척washed with brine
5. 5
   건조dried over anhydrous sodium sulphate
6. 6
   농축concentrated under reduced pressure
7. 7
   기타to afford the crude, which
8. 8
   기타was purified by column chromatography (using silica gel and 2% ethyl acetate in Hexane as eluent)

실험 절차

To a solution of 3-bromo-5-fluorophenol (0.5 g, 2.6 mmol) in DMF (4.5 mL) was added K2CO3 (0.9 g, 6.54 mmol) and stirred at 25° C. for 10 min. Water (0.5 mL) was added to the above mixture followed by addition of 2-Chloro-2,2,-difluoroacetic acid sodium salt (0.6 g, 3.93 mmol) and stirring was continued at 100° C. for 3 h. The reaction mixture was cooled to 25° C. and diluted with ethyl acetate, washed with brine, dried over anhydrous sodium sulphate and concentrated under reduced pressure to afford the crude, which was purified by column chromatography (using silica gel and 2% ethyl acetate in Hexane as eluent) to afford the desired compound (Int-45). 1H NMR (400 MHz, CDCl3) δ ppm 7.2-6.9 (2H, m), 6.8-6.7 (1H, d), 6.7-6.2 (1H, m).

출처