反应详情

0.7 g of 50% sodium hydride in an oil was added in small portions to a mixture of 1.9 g of 2,5-dimethylpyrazole 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 3 hours. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluted with ethyl acetate:ethanol=10:1 by volume). The product was recrystallized from isopropyl alcohol to obtain 0.8 g of the titled compound as colorless prisms having a melting point of 187°-190° C.

1. temperaturewas then heated on a water bath for 3 hours
2. distillationThe solvent was distilled off under reduced pressure
3. customthe residue was purified by silica gel column chromatography (eluted with ethyl acetate:ethanol=10:1 by volume)
4. customThe product was recrystallized from isopropyl alcohol