HCID 131711077, compound → HCID 252593, compound

Participants

Reaction Steps

The ergotoxine-benzene adduct formed in accordance with Example 7 in an amount of 50.0 g was hydrogenated in 0.7 liter of dioxane at 60° C at a hydrogen pressure of 50 atmospheres above atmospheric in a shaking or stirring autoclave provided with heating means in the presence of Raney nickel within a time of 2 hours. The solution of the formed 9,10-dihydroergotoxine was filtered off the catalyst and concentrated by evaporation to dryness in a vacuum. The hydrogenated base was then caused to crystallize out in ethylacetate at 4° C. The crystallizate was removed by suction and dried at 60° C. There were obtained 47.5 g (equal to 90% of the theoretical) tlc-pure white crystalline product in the form of the ergotoxine base with a degree of purity of 90%. The specific rotation was (α)D20 = -45.6° (c = 2 in pyridine).

Provenance & Evidence