反应详情

30 g (149 mmol) 1-chlorophthalazine (prepared from phthalazone in the manner described under Example 67A.1) and 20 g (157 mmol) 4-chloroaniline are heated in 630 ml n-butanol for 30 min to 65° C. The crude product is filtered off, washed with ether, taken up in 2 l di-chloromethane/methanol 9:1, and washed with sat. NaHCO3 solution and brine. The aqueous phases are extracted three times with dichloromethane/methanol 9:1, the organic phases dried (Na2SO4), and evaporated to a residual volume of ≈50 ml, leading to crystallization of the title compound: m.p.: 211° C.; Anal. calc.(C14H10N3Cl) C, 65.76%; H, 3.94%; N, 16.43%, Cl, 13.86%. found C, 66.02%; H, 3.92%; N, 16.53%, Cl, 13.51%.

1. filtrationThe crude product is filtered off
2. washwashed with ether
3. washwashed with sat. NaHCO3 solution and brine
4. extractionThe aqueous phases are extracted three times with dichloromethane/methanol 9:1
5. dry with materialthe organic phases dried (Na2SO4)
6. customevaporated to a residual volume of ≈50 ml
7. customleading to crystallization of the title compound