反应详情

温度

110 °C

Tris(dibenzylideneacetone)dipalladium (0.039 g) was added to a mixture of a 4:1 mixture (0.25 g) of 3-cyano-4-(6-iodo-2,3-methylenedioxyanilino)-6,7-dimethoxyquinoline and 3-cyano-4-(4,6-diiodo-2,3-methylenedioxyanilino)-6,7-dimethoxyquinoline (Example 10, Note [11]), zinc cyanide (0.092 g), diphenylphosphinoferrocene (0.046 g), zinc powder (0.017 g) and DMA (15 ml) and the resultant mixture was stirred and heated to 110° C. for 1 hour. The mixture was cooled to ambient temperature and partitioned between ethyl acetate and water. The organic layer was dried over magnesium sulphate and evaporated and the residue was purified by column chromatography on silica using increasingly polar mixtures of hexane and ethyl acetate as eluent. There were thus obtained in turn:—

1. temperatureThe mixture was cooled to ambient temperature
2. custompartitioned between ethyl acetate and water
3. dry with materialThe organic layer was dried over magnesium sulphate
4. customevaporated
5. customthe residue was purified by column chromatography on silica using
6. temperatureincreasingly polar mixtures of hexane and ethyl acetate as eluent
7. customThere were thus obtained in turn