http://rdf.ncbi.nlm.nih.gov/pubchem/patent/PL-433179-A1
Outgoing Links
| Predicate | Object |
|---|---|
| assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_1925630369470a4aa51694f659e2c4b2 |
| classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D471-04 |
| filingDate | 2020-03-09-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| inventor | http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_5f8c46e0b1a66c6e7154ab7e41ab4ca6 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_4136fa32eb06f0a16d7becefffe765b9 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_86978729d2db2dcbacbac72aeebf4640 |
| publicationDate | 2021-09-13-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| publicationNumber | PL-433179-A1 |
| titleOfInvention | 4,7-diiodo-1,10-phenanthroline and the method of its preparation |
| abstract | The subject of the invention is 4,7-diiodo-1,10-phenanthroline represented by the formula 1 and the method of its preparation, which consists in placing in the reactor, under an inert gas atmosphere, potassium iodide, then an aqueous solution of hydroiodic acid and an aqueous acid solution. phosphorus (I) (H3PO2), then 4,7-dichloro-1,10-phenanthroline is added and the mentioned reactants are mixed, with 2 to 20 moles of potassium iodide, 10 to 100 moles of hydroiodic acid, and 2 to 20 moles of H3PO2, followed by heating at 80 to 140 ° C for at least 4 hours under an inert gas atmosphere, and then After heating, the reaction mixture is cooled to a temperature of 10 to 40 ° C, and the separated precipitate of diiodophenanthroline dihydride is filtered off, preferably on a sintered glass filter, under reduced pressure, the filtered precipitate is further washed in a known manner, for example on a frit several times with ethanol or isopropane with olives or, most preferably, with methanol, in portions of 100 to 10,000 ml based on 1 mole of the substrate used for the reaction, i.e. 4,7-dichloro-1,10-phenanthroline, all of the dihydrochloride thus obtained is then placed in the reactor containing 15 to 150 moles of NaOH in the form of an aqueous solution, and from 2000 to 20,000 ml of dichloromethane, the given amounts of NaOH and dichloromethane refer to 1 mole of the substrate used in the reaction, and then additionally - based on 1 mole of substrate - from 0 , 01 to 0.5 mole of tetrabutylammonium chloride or tetrabutylammonium bisulfate or most preferably tetrabutylammonium hydroxide in the form of an aqueous solution with a concentration of at least 5% by mass, and the resulting reaction mixture is stirred vigorously at a temperature of 10 to 60 ° C for not less than 10 minutes, then, after turning off the stirrer from the two layers formed, the organic layer is separated, then washed with water several times, in portions of at least 25 0 ml, and dried with a drying agent used in an amount of at least 50 g, the above-mentioned amounts of washing water and drying agent are related to 1 mole of substrate, and in the next step volatile fractions are evaporated from the dried solution, and the residue is washed at least once, on the filter - first with ethanol or isopropanol or most preferably with methanol and then with a low-boiling liquid, saturated hydrocarbon or a mixture of liquid, saturated, low-boiling hydrocarbons, using up to five volumes of washing solvent based on the volume of the sediment, each time i.e. after washing with methanol, ethanol or isopropanol followed by a low boiling liquid saturated hydrocarbon or a mixture of liquid saturated low boiling hydrocarbons, the precipitate is filtered under reduced pressure in the usual manner and finally the residue of the volatile fractions is removed under a reduced pressure of not more than 50 mmHg, at a temperature of 20 to 100 ° C for at least 1 hour, thereby obtaining 4,7-diiodo-1,10-phenanthroline,> 98% pure, as a white solid in yield up to 65%. |
| priorityDate | 2020-03-09-04:00^^<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: 38.