反应详情

A solution of 2 ml boron tribromide (≈1M in CH2Cl2) is mixed with a suspension of 0.19 g (0.50 mmol) 1-(4-chloro-3-methoxyanilino)-4-(4-pyridylmethyl)phthalazine (Example 68B) in 4 ml dichioromethane at 0° C. under a nitrogen atmosphere. The resinous mixture is left to stand for 18 h at RT, the dichloromethane phase is then decanted, and the glutinous residue stirred with 10 ml THF and 5 ml sat. NaHCO3 solution. The resulting suspension is filtered, the filter residue washed with THF and discarded. The THF phase is separated and dried (Na2SO4), concentrated by evaporation, chromatographed (SiO2; acetate/CH3OH 40:1→19:1) and title compound crystallized from acetonitrile/methanol: m.p.: 245-246° C.; HPLC: tRet(Grads5-40)=8.8; FAB MS (M+H)+=363.

1. waitThe resinous mixture is left
2. customthe dichloromethane phase is then decanted
3. filtrationThe resulting suspension is filtered
4. washthe filter residue washed with THF
5. customThe THF phase is separated
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated by evaporation
8. customchromatographed (SiO2; acetate/CH3OH 40:1→19:1) and title compound
9. customcrystallized from acetonitrile/methanol