http://rdf.ncbi.nlm.nih.gov/pubchem/patent/GB-478330-A

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assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_28fd8a2f7ca983e63d38bcf83d182d44
filingDate 1936-04-08-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1938-01-17-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-478330-A
titleOfInvention Process for the preparation of a new ergot alkaloid and its salts
abstract A new alkaloid, called ergobasine, is obtained from ergot by taking advantage of its relatively great solubility in water and its sparing solubility in chlorinated aliphatic hydrocarbons. Thus, the finely-powdered ergot is ground with water and the filtered solution, preferably after concentration in vacuo, is shaken with a large quantity of a chlorinated hydrocarbon, whereupon the extract is concentrated to allow the new alkaloid to crystallize out. Again, an aqueous acid extract of ergot is treated with an alkali such as sodium bicarbonate and then shaken with a chlorinated aliphatic hydrocarbon such as chloroform; the first extracts contain the alkaloids of the ergotoxine-ergotamine group, whilst the later extracts contain the new alkaloid. The new alkaloid is stated to be distinguished from ergometrine by the physical and chemical properties both of itself and its salts. According to the examples: (1) a benzene extract of ergot, prepared according to German Specification 357,272, is concentrated and the alkaloids precipitated by petroleum ether; the dried mixture is then ground with cold water and the united extracts shaken with a large quantity of chloroform; the new alkaloid is isolated by evaporation in vacuo of the solution, recrystallized from benzene and converted into its tartrate; (2) the benzene extract of (1) is concentrated, the alkaloids separating out are dissolved in a large quantity of chloroform and the solution allowed to stand in an ice box, when the new alkaloid separates out; after purification by recrystallization from benzene or from di- or tri-chlorethylene, it is converted into its hydrochloride; (3) a concentrated fluid extract of secale cornutum, which has been repeatedly concentrated in vacuo and the precipitate removed, is made alkaline with sodium bicarbonate solution and the aqueous filtrate extracted with large quantities of chloroform; the extract is treated with dilute sulphuric acid, the acid solution neutralized with sodium bicarbonate solution and the new alkaloid obtained by further extraction with chloroform; (4) an aqueous hydrochloric acid extract of ergot is neutralized with sodium bicarbonate, the concentrated filtrate extracted with a large quantity of chloroform and the isolated alkaloid, after recrystallization from dichlorethylene, converted into its hydrobromide; (5) a tincture from secale cornutum is freed from alcohol by low temperature distillation under reduced pressure, sodium bicarbonate solution added to the concentrated filtrate, and the new base extracted from the filtered solution by means of chloroform.
priorityDate 1935-04-11-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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