反应详情

Under N2 atmosphere, in an ampoule 1.8 g (12.7 mMol) of trans 4-isopropyl-cyclohexylamine (preparation see Arzneim. Forsch. 1969, 19, 140) and 700 mg (2.4 mMol) of 1-chloro-4-[6-methoxy-pyridin-3-yl)methyl]phthalazine are heated during 14 h at 140° C. The suspension is dissolved by dilution with EtOAc, 1.5 ml of NH3 solution (25%) and water, and the aqueous phase is removed and extracted twice with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and evaporated. Crystallization from EtOAc/hexane 1:1 results in the title compound: M.p. 124-125° C.; FAB-MS: (M+H)+=391; HPLC(Grad20-100) tRet12.4.

1. customthe aqueous phase is removed
2. extractionextracted twice with EtOAc
3. washThe organic phases are washed with water and brine
4. dry with materialdried (Na2SO4)
5. customevaporated
6. customCrystallization from EtOAc/hexane 1:1