Hydrochloric Acid → HCID 178514928, compound

Participants

Reaction Steps

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.

Provenance & Evidence