반응 #85138

반응 방정식

2,2,2-trifluoroethyl trifluoromethanesulphonate

potassium carbonate

2,2,2-trifluoroethyl trifluoromethanesulphonate

4-iodo-6-methoxypyridin-3-ol

water ethyl acetate

→

4-Iodo-2-methoxy-5-(2,2,2-trifluoroethoxy)pyridine

용매

dimethylformamide

acetonitrile

반응 조건

후처리

1. 1
   기타the mixture was irradiated in a microwave at 150° C. for 30 min
2. 2
   기타the reaction mixture was once more irradiated in the microwave at 150° C. for 30 min
3. 3
   추출the aqueous phase was extracted twice with ethyl acetate
4. 4
   세척The combined organic phases were washed with saturated aqueous sodium chloride solution
5. 5
   건조dried (sodium sulphate)
6. 6
   여과filtered
7. 7
   농축concentrated under reduced pressure
8. 8
   기타dried

실험 절차

466 mg (3.4 mmol, 2.0 eq.) of potassium carbonate and 567 mg (2.5 mmol, 1.5 eq.) of 2,2,2-trifluoroethyl trifluoromethanesulphonate were added to a solution of 455 mg (purity 93%, 1.7 mmol) of 4-iodo-6-methoxypyridin-3-ol in 10 ml of dimethylformamide and 0.4 ml of acetonitrile, and the mixture was irradiated in a microwave at 150° C. for 30 min. A further 393 mg (1.7 mmol, 1.0 eq.) of 2,2,2-trifluoroethyl trifluoromethanesulphonate were added, and the reaction mixture was once more irradiated in the microwave at 150° C. for 30 min. After addition of water/ethyl acetate and phase separation, the aqueous phase was extracted twice with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried (sodium sulphate), filtered, concentrated under reduced pressure and dried. Yield: 500 mg (purity 94%, 94% of theory)

출처