反应详情

1.0 g of 50% sodium hydride in an oil was added in small portions to a mixture of 2.0 g of imidazole and 20 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 3 hours. After allowing the mixture to cool, ice-water was added to the reaction mixture, and the precipitated crystals were filtered and washed with water. The crystals thus obtained were dissolved in ethanol, and the solution was concentrated to a volume of about 1/3, followed by allowing to cool to obtain 1.3 g of the titled compound as colorless prisms having a melting point of higher than 260° C. (with decomposition).

1. temperaturewas then heated on a water bath for 3 hours
2. temperatureto cool
3. filtrationthe precipitated crystals were filtered
4. washwashed with water
5. customThe crystals thus obtained
6. concentrationthe solution was concentrated to a volume of about 1/3
7. temperatureto cool