反应详情

A solution of 1.0 g (2.97 retool) of 1-benzyl-3 -bromo-7-chloro-2-methylpyrrolo [2,3-d]pyridazine in 5 ml of benzylamine is heated to 150° C. for 5 h and subsequently cooled to room temperature. The solution is then treated with 50 ml of water, adjusted to pH 6 with 2 N hydrochloric acid and extracted with 2×50 ml of dichloromethane. The organic extracts are dried over magnesium sulfate and concentrated. The residue which remains is chromatographed on silica gel (eluent: toluene/dioxane=2:1). After concentration of the fractions of Rf=0.25 and crystallization from diisopropyl ether, 1.01 g (84%) of the title compound are isolated. M.p.: 185°-188° C.

1. extractionextracted with 2×50 ml of dichloromethane
2. dry with materialThe organic extracts are dried over magnesium sulfate
3. concentrationconcentrated
4. customThe residue which remains is chromatographed on silica gel (eluent: toluene/dioxane=2:1)
5. customAfter concentration of the fractions of Rf=0.25 and crystallization from diisopropyl ether, 1.01 g (84%) of the title compound
6. customare isolated