反应详情

To an 8 ml dimethylformamide solution of 300 mg of the compound (4) synthesized in Reference Example 4 were added 93 mg of chloroacetonitrile, 355 mg of sodium iodide, and 196 mg of potassium carbonate. This was then heated at reflux for 2 hours. To the reaction was added 10 ml of ice water, then extraction was performed with ethyl acetate. The extract was dried, filtered, then concentrated under reduced pressure to obtain a residue which was then purified by silica gel column chromatography (methylene chloride:methanol =30:1) to obtain the above-identified compound (26) in an amount of 313 mg (yield of 91%).

1. temperatureThis was then heated
2. temperatureat reflux for 2 hours
3. extractionextraction
4. customThe extract was dried
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customto obtain a residue which
8. customwas then purified by silica gel column chromatography (methylene chloride:methanol =30:1)