反应详情

To an ice-cold suspension of Oxone® (525 mg, 854 μmol, CAS RN 10058-23-8) in methanol (0.6 mL) and water (0.6 mL) was added dropwise a solution of 2-methylsulfanyl-6-trifluoromethyl-isonicotinic acid (0.09 g, 341 μmol) in methanol (1.2 mL) and the reaction mixture was stirred in an ice-bath for 2 hours. After stirring at room temperature for another 4.5 hours the reaction mixture was poured on 10% aqueous citric acid solution and EtOAc and the layers were separated. The aqueous layer was extracted twice with EtOAc and the organic layers were washed with water, 10% aqueous Na2S2O3 solution and brine, dried over MgSO4, filtered, and evaporated. Colorless solid (0.106 g; 98%). MS (ESI): m/z=267.99 [M−H]−. This material was used in the next step without further purification.

1. stirringAfter stirring at room temperature for another 4.5 hours the reaction mixture
2. customthe layers were separated
3. extractionThe aqueous layer was extracted twice with EtOAc
4. washthe organic layers were washed with water, 10% aqueous Na2S2O3 solution and brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated
8. customThis material was used in the next step without further purification