Water → HCID 58379057, compound

Participants

Reaction Steps

Heat a mixture of 1,4-dichlorophthalazine (10.0 g, 50.2 mmol), (S)-tert-butyl 3-methylpiperazine-1-carboxylate (15.1 g, 75.4 mmol) and triethylamine (21.0 mL, 150.7 mmol) in DMSO (200 mL) at 120° C. for 2 d. Pour the reaction mixture into water, rinsing with CH2Cl2. Extract with Et2O. Wash the organic layer with water (2×), dry over Na2SO4, and concentrate under reduced pressure. Purify the resulting residue by flash silica gel chromatography (gradient of 0 to 20% EtOAc in CH2Cl2) to provide the title compound as a pale yellow solid (6.0 g, 33%). ES/MS m/z (35Cl) 363.0 (M+1).

Provenance & Evidence