Potassium Carbonate → HCID 178505239, compound

Participants

Reaction Steps

Methanesulphonic anhydride (1.55 g) was added to a stirred mixture of 4-hydroxy-7-trifluoromethoxy-quinoline-1-oxide (2.0 g), potassium carbonate (1.2 g) and dichloromethane (100 ml) at 0°. After stirring at 0° for a further 2.5 hours, the reaction mixture was washed with saturated aqueous sodium carbonate (60 ml) and the dichloromethane phase separated. The aqueous phase was extracted with dichloromethane (2×50 ml) and the combined dichloromethane phase and extracts were dried over magnesium sulphate. The solvent was removed by evaporation and water (100 ml) followed by saturated aqueous sodium bicarbonate (5 ml) at 10° was added. The solid was collected by filtration to give the novel compound 4-hydroxy-7-trifluoromethoxyquinol-3-yl methanesulphonate, m.p. 125°-127°.

Provenance & Evidence