反应详情

In a pressure bottle was placed 2-chloro-1-pyrimidin-2-ylethanol (3.525 g, 22.24 mmol), sodium iodide (0.344 g, 2.29 mmol) and a 2M. methylamine solution (160 ml, 320 mmol) in methanol. The bottle was sealed and heated at 62° for 17 hr. The solvent was evaporated and the residue stirred with 10% MeOH—CHCl3. Filtration and evaporation gave a dark oil that was chromatographed over silica gel (90 g) eluting with 5-10% MeOH—CH2Cl2 containing 1% triethylamine The product was obtained as an amber oil (1.625 g).

1. customThe bottle was sealed
2. temperatureheated at 62° for 17 hr
3. customThe solvent was evaporated
4. filtrationFiltration and evaporation
5. customgave a dark oil that
6. customwas chromatographed over silica gel (90 g)
7. washeluting with 5-10% MeOH—CH2Cl2 containing 1% triethylamine The product