反应详情

1.7 g of 50% sodium hydride in an oil was added in small portions to a mixture of 5.1 g of tetrazole and 30 ml of dimethylformamide, and the resulting mixture was stirred for 30 minutes. 3.0 g of 6-methylergolin-8β-ylmethyl tosylate was added to the mixture which was then heated on a water bath for 11 hours. The solvent was distilled off under reduced pressure, and the residue was purified by alumina column chromatography (eluted with acetone). The product was recrystallized from acetone to obtain 0.7 g of the titled compound as colorless needles having a melting point of 206°-209° C.

1. temperaturewas then heated on a water bath for 11 hours
2. distillationThe solvent was distilled off under reduced pressure
3. customthe residue was purified by alumina column chromatography (eluted with acetone)
4. customThe product was recrystallized from acetone