反应详情

A mixture of ethyl 6-chloro-3-pyridazinecarboxylate (0.29 g, 1.55 mmol, Example 1, Step A) and dimethyl 4-aminoisophthalate (0.36 g, 1.72 mmol, Example 1, Step B) was heated as a melt at 165°-170° C. for 30 min. The oil was dissolved into chloroform, washed with 10% ammonium hydroxide solution, dried (MgSO4) , filtered and concentrated. Medium pressure chromatography (silica gel, chloroform to 1% methanol in chloroform) of the crude oily-solid afforded 2-ethyl 8-methyl 10-oxo-10H-pyridazino[6,1-b]quinazoline-2,8-dicarboxylate as a yellow solid, mp 218°-221° C. dec.

1. temperaturewas heated as a melt at 165°-170° C. for 30 min
2. washwashed with 10% ammonium hydroxide solution
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated