反应详情

温度

100 °C

A solution of 3-bromo-4-hydroxy-1-phenyl-1,8-naphthyridin-2(1H)-one (1 g) in a mixture of 2,6-lutidine (5 mL) and 4-hydroxy-piperidine (3.12 g) was heated at 100° C. for 32 hours. The lutidine was removed by evaporation under high vacuum. The residue was dissolved in CH2CN(20): H2O(80): CH3CO2H(1) and separated by reversed phase preparative HPLC (Whatman Magnum 40 with Partisil 40/ODS-3). The fractions containing the desired product were combined and evaporated to yield a partially crystalline material which was recrystallized from isopropanol to yield the desired product, m.p. 256°-258° C.

1. customThe lutidine was removed by evaporation under high vacuum
2. dissolutionThe residue was dissolved in CH2CN(20)
3. customH2O(80): CH3CO2H(1) and separated by reversed phase preparative HPLC (Whatman Magnum 40 with Partisil 40/ODS-3)
4. additionThe fractions containing the desired product
5. customevaporated
6. customto yield a partially crystalline material which
7. customwas recrystallized from isopropanol