反应详情

To a solution of t-butyl hypochlorite (3.8 g., 0.038 m.) in acetone (200 ml.), which was cooled to -60°, is added the sodium salt of phthalhydrazide (4.8 g., 0.021 g.). After 2.5 hours at -60° to -50°, the resulting green reaction mixture is filtered to give a solution of 1,4-phthalazinedione. Cyclopentadiene (2.0 ml. ) is added to the cooled green solution (-50°) and white crystals precipitate almost immediately. After 10 minutes at -50°, the crude product (3.0 g.) is collected by filtration. Recrystallization from CH2Cl2 /Et2O affords white microprisms of 1,4-methano-1,4-dihydropyridazino[1,2-b]phthalazine-6,11-dione (1.8 g., 64%), mp 206°-212° C.

1. filtrationthe resulting green reaction mixture is filtered