反应详情

A mixture of 4-hydroxy-7-trifluoromethyl-quinoline-1-oxide (2.0 g), methanesulphonic anhydride (1.7 g) and potassium carbonate (1.3 g) in dichloromethane (100 ml) was stirred at 0° for 2 hours. Further methanesulphonic anhydride (1.7 g) and potassium carbonate (1.3 g) were then added and the mixture was stirred at ambient temperature overnight. Water (50 ml) was added and the precipitated solid collected by filtration to give a first crop of the novel compound 4-hydroxy-7-trifluoromethylquinol-3-yl methanesulphonate, m.p. 220°. The dichloromethane layer of the filtrate was separated and the aqueous layer subsequently extracted with dichloromethane (2×25 ml). The combined dichloromethane layer and extracts were evaporated to dryness. The residue was purified by flash chromatography on a silica gel column eluted with dichloromethane:methanol (20:1) to give a second crop of 4-hydroxy-7-trifluoromethylquinol-3-yl methanesulphonate, m.p. 220°.

1. stirringthe mixture was stirred at ambient temperature overnight
2. filtrationthe precipitated solid collected by filtration