反应详情

0.4 g of 50% sodium hydride in an oil was added in small portions to a mixture of 2.0 g of 1,2,4-triazole and 20 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 1 hour. After allowing the mixture to cool, water was added to the reaction mixture, and the precipitated crystals were separated by filtration, washed with water and purified by alumina column chromatography (eluted with dichloromethane). The product was recrystallized from methanol to obtain 0.8 g of the titled compound as colorless needles having a melting point of 245°-253° C.

1. temperaturewas then heated on a water bath for 1 hour
2. temperatureto cool
3. customthe precipitated crystals were separated by filtration
4. washwashed with water
5. custompurified by alumina column chromatography (eluted with dichloromethane)
6. customThe product was recrystallized from methanol