反应详情

Heat a mixture of 1-chloro-4-(4-fluorophenyl)phthalazine (5.02 g, 19.4 mmol), (S)-tert-butyl 2-ethylpiperazine-1-carboxylate (5.00 g, 23.3 mmol) and K2CO3 (5.38 g, 38.9 mmol) in DMSO (75 mL) at 120° C. for 1 d. Pour the reaction mixture into water, rinsing with EtOAc. Extract with EtOAc. Wash the organic layer with water (2×), then brine, dry over Na2SO4, and concentrate under reduced pressure. Purify the resulting residue by flash silica gel chromatography (gradient of 20 to 80% EtOAc in hexanes) to provide the title compound (5.11 g, 60%). ES/MS m/z 437.2 (M+1).

1. temperatureHeat
2. washrinsing with EtOAc
3. extractionExtract with EtOAc
4. washWash the organic layer with water (2×)
5. dry with materialbrine, dry over Na2SO4
6. concentrationconcentrate under reduced pressure
7. customPurify the resulting residue by flash silica gel chromatography (gradient of 20 to 80% EtOAc in hexanes)