反应详情

0.68 g of 50% sodium hydride in an oil was added in small portions to a mixture of 2.1 g of 2-propylimidazole and 50 ml of dimethylformamide, and the resulting mixture was stirred for 30 minutes. 2.0 g of 6-methylergolin-8β-ylmethyl tosylate was added to the mixture which was then heated on a water bath for 2.5 hours. The solvent was distilled off under reduced pressure, and the residue was purified by alumina column chromatography (eluted with ethyl acetate:benzene=1:2, and then with ethyl acetate). The resulting product was recrystallized from acetone-hexane to obtain 0.8 g of the titled compound as colorless needles having a melting point of 223°-227° C. (with decomposition).

1. temperaturewas then heated on a water bath for 2.5 hours
2. distillationThe solvent was distilled off under reduced pressure
3. customthe residue was purified by alumina column chromatography (
4. washeluted with ethyl acetate
5. customThe resulting product was recrystallized from acetone-hexane