반응 #717591

반응 방정식

methanol

4-amino-2,5-difluorobenzonitrile

→

title compound

수율 97.0%

4-amino-5-fluoro-2-methoxybenzonitrile

수율 97.0%

용매

tetrahydrofuran

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGThe reaction mixture was stirred at 70° C. for 3 hours
2. 2
   기타The solvent was partially removed
3. 3
   workup.ADDITIONether was added into the mixture
4. 4
   세척The organic layer was washed with bicarbonate and brine
5. 5
   기타dried
6. 6
   여과filtered
7. 7
   기타The organic solvent was removed under reduced pressure

실험 절차

To a mixture of methanol (10.48 mL, 0.25 mol) and anh. tetrahydrofuran (60 mL) was added dropwise a solution of potassium tert-butilate (6.76 g, 0.05 mol) in anh. tetrahydrofuran (52 mL) at 0° C. under nitrogen atmosphere. The mixture was stirred for minutes at room temperature and then 4-amino-2,5-difluorobenzonitrile (4 g, 0.02 mol) was added. The reaction mixture was stirred at 70° C. for 3 hours. The solvent was partially removed and ether was added into the mixture. The organic layer was washed with bicarbonate and brine, dried and filtered. The organic solvent was removed under reduced pressure to give the title compound as a yellow solid (97%), which was used in the next step without further purification.

출처