Phthalazine → HCID 10200902, compound

Participants

Reaction Conditions

Reaction Steps

Under N2 atmosphere, 0.40 g (2.7 mMol) of 4-tert-butyl-aniline and 0.62 ml 4 N HCl/dioxane are added to 750 mg (2.6 mMol) of 1-chloro-4-[6-methoxy-pyridin-3-yl)methyl]phthalazine in 11 ml of methanol, and the mixture is stirred for 2 h at 65° C. After cooling, the resulting yellow solution is diluted with EtOAc, 20 ml of water and 10 ml of 2.5% NH3 solution, and the aqueous phase is removed and extracted twice with EtOAc. The organic phases are washed with water and brine, dried and partially evaporated with a RE. After addition of DIPE to the remnant, the title compound crystallizes out: FAB-MS: (M+H)+=399; HPLC(Grad20-100) tRet=11.9.

Provenance & Evidence