http://rdf.ncbi.nlm.nih.gov/pubchem/patent/GB-717281-A
Outgoing Links
Predicate | Object |
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assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_14effe3850d2129f863b969dac4f1db8 |
classificationCPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C237-26 |
filingDate | 1952-07-01-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationDate | 1954-10-27-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationNumber | GB-717281-A |
titleOfInvention | Improvements relating to the purification of chlortetracycline-containing material |
abstract | Chlortetracycline-containing material is purified by reacting the same in water at a pH not exceeding 3, with an anionic organic sulphuric acid derivative of formula R-On-SO2OH, in which n is 1 or zero, and R is a hydrophobic organic radical such as alkyl, aryl, aralkyl, alkaryl, haloaryl or azoaryl, in which the attaching valence load is linked to a carbon atom, the molecular weight being not less than 210, recovering the resulting chlortetracycline salt-type compound of said sulphuric acid derivative and, if desired, converting the same to another form of chlortetracycline, e.g. hydrochloride, base or calcium salt. It is preferred to use excess of the sulphuric acid derivative, and to carry out the reaction in the presence of a water-immiscible solvent for the chlortetracycline salt-type compound of said sulphuric acid derivative. Reactants added in any order; preferred pH 1-2, at which pH, salts of the above sulphuric acid derivatives are converted to the free acid. Solvents evaporated at a temperature not exceeding 60 DEG C. Chlortetracycline compound may be further purified by recrystallization from an organic solvent. The chlortetracycline-containing material refers to chlortetracycline in any form, e.g. neutral, i.e. free base, salts with acids, e.g. hydrochloride, salts with metals, e.g. sodium. It may be obtained by acidifying a fermentation broth and filtering off the insolubles; or by extracting with aqueous acid the precipitate formed by adding alkali to a fermentation broth. Such solutions may be treated with activated carbon. Specified sulphuric acid derivatives are: sodium tetradecylsulphate; sodium di-(2-ethyl hexyl) sulphosuccinate; sodium 2-ethyl heptyl sulphate; sodium lauryl sulphate; 2,5-dichlorobenzene sulphonic acid; p-xylene sulphonic acid; 4-hydroxyazobenzene 41-sulphonic acid; 2,4-dinitronaphthol-7-sulphonic acid; 5-sulphosalicylic acid; 2,4-dichlorophenol-6-sulphonic acid; 2 - chlorotoluene - 5 - sulphonic acid; 4 - nitrochlorobenzene - 2 - sulphonic acid; 2 - naphthalenesulphonic acid; 2,4 - dihydroxy azobenzene 4-sulphonic acid; salts of the above acids; turkey red oil; alkyl sulphates having 10 to 20 C atoms; aryl, aralkyl or alkaryl sulphonic acids having 10 to 25 C atoms; and sodium 2,9-diethyltridecane-6-sulphate. Specified water-immiscible solvents are: halogenated hydrocarbons such as ethylene dichloride, trichloroethylene, trichloroethane, propylene dichloride, chloroform, 2-phenoxy ethanol, dimethyl phthalate, ethyl hydrogen phthalate, isopropyl acetate, butyl acetate, ethers, e.g. dichloroisopropyl ether, ketones such as methyl isobutyl ketone, alcohols of 4 or more C atoms, e.g. methylisobutyl carbinol, hexanols, butanol and amyl alcohol. Specification 690,381 is referred to. |
isCitedBy | http://rdf.ncbi.nlm.nih.gov/pubchem/patent/US-2988569-A |
priorityDate | 1951-07-11-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
type | http://data.epo.org/linked-data/def/patent/Publication |
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Total number of triples: 81.