反应详情

Under exclusion of air, 200 mg (0.78 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine (Example 67A.1), 173 mg (1.25 mmol) K2CO3, and 120 mg (0.94 mmol) 3-chlorophenol (Fluka) are heated in 2 ml DMSO for 3 h to 90° C. The reaction mixture is distributed between 20 ml water and 20 ml ethyl acetate, and the aqueous phase separated and extracted with 2 portions of ethyl acetate. The organic phase is washed with water and brine, dried (MgSO4), and concentrated by evaporation. The residue is dissolved in ≦15 ml THF, precipitated with hexane, and filtered. Title compound is obtained from the evaporated filtrate after chromatography (SiO2; ethyl acetate/CH3OH, 4:1): m.p.: 143-145° C.; HPLC: tRet(Grad20-100)=8.9; FAB MS (M+H)+=348.

1. customthe aqueous phase separated
2. extractionextracted with 2 portions of ethyl acetate
3. washThe organic phase is washed with water and brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated by evaporation
6. dissolutionThe residue is dissolved in ≦15 ml THF
7. customprecipitated with hexane
8. filtrationfiltered