反应详情

温度

155 °C

A mixture of 5-hydroxyisoquinoline (2.05 g, 14.1 mmol), ethylene carbonate (1.43 g, 16.2 mmol), K2CO3 (0.97 g, 7.1 mmol) in DMF (6 mL) was heated at 155° C. for 1.5 h under stirring in a sealed tube. After cooling, the mixture was diluted with CHCl3 and filtered through a pad of Celite. The brownish filtrate was concentrated in vacuo, and the residue was purified by chromatography on silica gel using EtOAc as eluent to give 1.8 g (67%) of the title product as a beige oil which solidified on standing: mp 64-67° C., HRMS m/z calcd for C11H11NO2 (M)+ 189.0790, found 189.0789. Anal. (C11H11NO2) C, H, N.

1. temperatureAfter cooling
2. filtrationfiltered through a pad of Celite
3. concentrationThe brownish filtrate was concentrated in vacuo
4. customthe residue was purified by chromatography on silica gel