http://rdf.ncbi.nlm.nih.gov/pubchem/patent/GB-438515-A

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assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_a27ca344c4cbf344abe5af956ed2d12f
classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/A61K31-56
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/A61K31-56
filingDate 1934-05-07-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1935-11-07-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-438515-A
titleOfInvention A method of purifying crude extracts of the germinal gland hormones and of isolating the latter therefrom
abstract Germinal gland hormones are isolated from extracts containing them by treating said extracts with acylating agents under anhydrous conditions, separating the esterified products from the non-esterified parts by physical methods, saponifying the purified esters and isolating the hormones. The process is applied particularly to the purification of male hormone and to the separation of mixtures of various hormones and like substances such as pregnandiol. The physical methods used for isolating the esterified hormones include fractional crystallization from dilute alcohol or dilute acetone, fractional distillation in very high vacuum, and extraction with pure organic solvents such as alcohol, ethyl acetate or acetone. Acylating agents referred to are acetic anhydride, phthalic anhydride, p-toluene sulphonic acid chloride, anthraquinone-2-carboxylic acid chloride and salicylic acid chloride. When acid chlorides are used the reaction may take place in presence of an agent such as pyridin serving to combine with the hydrochloric acid produced. The hormone-containing extracts employed may be prepared from urine or from organs, and may be crude or may have been pre-treated by known purifying processes. According to examples: (1) an extract from male urine is treated with toluene sulphochloride in solution in toluene containing also pyridin, the precipitated pyridin hydrochloride is removed and the esterified products separated and saponified; (2) an extract from the urine of pregnant women is acylated as in (1) and a fraction obtained by distillation is saponified, the saponification solution is largely diluted and extracted with ether, the ethereal extract is shaken with concentrated alkali hydroxide to remove follicle hormone and is then concentrated by evaporation so that pregnandiol separates in crystals and the male hormone remains as an oily residue; follicle hormone hydrate remaining in the saponification liquid when the latter is extracted by ether is recovered by neutralizing with CO2 and extraction with ether. Specifications 432,435, 432,474, and 432,851 are referred to. Reference has been directed by the Comptroller to Specification 391,686.ALSO:A product obtained by acylating an extract of urine and separating the esters produced from non-esterified products is treated to obtain the individual hormones by a process comprising saponification by means of alkali, extraction of the diluted alkaline solution with ether, shaking the ethereal extract with concentrated alkali hydroxide solution to extract follicle hormone, concentrating the remaining ethereal extract to cause separation of pregnandiol crystals and finally to leave the male hormone as an oily residue, and recovery of follicle hormone hydrate from the initial alkaline saponification liquid by neutralization with carbon dioxide and extraction with ether. Specifications 432,435, 432,474, and 432,851 are referred to. Reference has been directed by the Comptroller to Specification 391,686.
priorityDate 1934-05-07-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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