反应详情

1.03 g of trimethyltin azide was added to 1.07 g of 2-(7-chloroquinolin-2-yl)methoxy-8-cyano-11-oxo-6,11-dihydrodibenz[b,e]oxepine obtained by the same method as in Reference example 34 suspended in 30 ml of xylene and the mixture was refluxed under heating for 13 hours. 1 ml of conc. hydrochloric acid was added to the reaction mixture, the mixture was adjusted to about pH 4 with a 1N-sodium hydroxide aqueous solution and crystals precipitated were collected by filtration. The crystals were dissolved in a chloroform-methanol mixed solution and the organic layer was washed with a saturated saline solution and then dried over anhydrous sodium sulfate. The residue obtained by removing the solvent was applied to silica gel column chromatography to obtain 1.25 g of the title compound.

1. customobtained by the same method as in Reference example 34
2. temperaturethe mixture was refluxed
3. temperatureunder heating for 13 hours
4. customprecipitated
5. filtrationwere collected by filtration
6. dissolutionThe crystals were dissolved in a chloroform-methanol mixed solution
7. washthe organic layer was washed with a saturated saline solution
8. dry with materialdried over anhydrous sodium sulfate
9. customThe residue obtained
10. customby removing the solvent