反应详情

温度

60 °C

Under N2 atmosphere, 0.35 ml (2.6 mMol) of Me3Sil are added to 500 mg (1.3 mMol) of trans 1-(4-isopropyl-cyclohexylamino)-4-[6-methoxy-(pyridin-3-yl)-methyl]-phthalazine in 15 ml of chloroform, followed by stirring for 16 h at 60° C. After cooling to RT, 15 ml of sat. NaHCO3 solution, 10 ml of water, EtOAc and a small amount of methanol are added, followed by agitation. From the resulting solution, the aqueous phase is removed and extracted twice with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and evaporated to dryness. Crystallization by partial evaporation of a solution in methanol results in the title compound: M.p. 271-272° C. (decomposition); FAB-MS: (M+H)+=377; HPLC(Grad20-100) tRet=10.2.

1. temperatureAfter cooling to RT
2. customFrom the resulting solution, the aqueous phase is removed
3. extractionextracted twice with EtOAc
4. washThe organic phases are washed with water and brine
5. dry with materialdried (Na2SO4)
6. customevaporated to dryness
7. customCrystallization
8. customby partial evaporation of a solution in methanol