反应详情

温度

60 °C

Under N2-atmosphere, 0.28 ml (2.05 mMol) Me3Sil are added to 400 mg (1.02 mMol) of trans 1-(4-isopropyl-cyclohexylamino)-4-[2-methoxy-(pyridin-4-yl)-methyl]-phthalazine in 10 ml chloroform, and the resulting mixture is stirred during 20 h at 60° C. After cooling to RT, 5 ml sat. NaHCO3-solution, 5 ml water, 20 ml EtOAc and a small amount of methanol are added, followed by agitation. The resulting white crystals are filtered off, washed with water and dried, yielding the title compound: M.p. 266-267° C. (decomposition); FAB-MS: (M+H)+=377; HPLC(Grad20-100) tRet=10.3). From the filtrate, by extraction with EtOAc, washing of the organic phase with water and brine, drying (Na2SO4), evaporation and crystallisation from dichlormethane/methanol under addition of ether, more product results.

1. temperatureAfter cooling to RT
2. filtrationThe resulting white crystals are filtered off
3. washwashed with water
4. customdried