反应详情

A mixture of 4-hydroxyquinoline-1-oxide (1 g), methanesulphonic anhydride (2 g) and potassium carbonate (2 g) in dichloromethane (20 ml) was stirred at 0° for 4 hours. Water (20 ml) was added to the mixture and the dichloromethane layer separated. The aqueous layer was extracted with dichloromethane (2×60 ml). The combined dichloromethane layer and extracts were dried over magnesium sulphate and evaporated to give a gum which was purified by flash chromatography on a silica gel column eluted with dichloromethane:methanol (19:1) to give the novel compound 4-hydroxyquinol-3-yl methanesulphonate, m.p. 224°.

1. customthe dichloromethane layer separated
2. extractionThe aqueous layer was extracted with dichloromethane (2×60 ml)
3. dry with materialThe combined dichloromethane layer and extracts were dried over magnesium sulphate
4. customevaporated
5. customto give a gum which
6. customwas purified by flash chromatography on a silica gel column
7. washeluted with dichloromethane:methanol (19:1)