反应详情

To a solution of t-butyl hypochlorite (12.3 g., 0.12 m.) in acetone (500 ml.), which is cooled to -50°, is added to sodium salt of phthalhydrazide (12.4 g., 0.067 m.). The reaction mixture is stirred vigorously for 3 hours at -50° and then filtered to give a solution of 1,4-phthalazinedione. 1,3-Cyclooctadiene (12.0 g., 0.11 m.) is added to the green solution (-50°) and the green solution is warmed to 0°. The solution is kept at 0° until the green color is discharged (1.5 hours). The crude product (5.6 g.) is collected by filtration. Recrystallization of the crude product from methylene chloride-methanol affords white microprisms of 1,4-butano-1,4-dihydropyridazino[1,2-b]phthalazine-6,11-dione (5.0 g., 53%) mp 206°-207° C.

1. filtrationfiltered