http://rdf.ncbi.nlm.nih.gov/pubchem/patent/PL-433281-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/C07C69-76 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C67-343 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C15-20 |
| filingDate | 2020-03-18-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| inventor | http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_d8c23b68670ab72678a0713b9892bb9b http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_5f8c46e0b1a66c6e7154ab7e41ab4ca6 |
| publicationDate | 2021-09-20-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| publicationNumber | PL-433281-A1 |
| titleOfInvention | 1,2-di (methoxycarbonyl) benzo [1,2-j] coronene and the method of its preparation |
| abstract | The subject of the invention is 1,2-di (methoxycarbonyl) benzo [1,2-j] coronene represented by the formula 1. The invention also relates to the method of obtaining 1,2-di (methoxycarbonyl) benzo [1,2-j] coronene represented by the formula 1 , consisting in the fact that in the first stage, perylene and dienophile in the form of dimethyl acetylenedicarboxylate are introduced into the reactor under an inert gas atmosphere, the excess of dienophile being at least three times, and then the reactor is closed and the reaction mixture contained therein is heated by at least 6 hours at a temperature not lower than 160 ° C but not higher than the decomposition temperature of the reaction mixture, then excess acetylenedicarboxylate is distilled off, and the residue is purified by column chromatography on silica gel using a low-boiling saturated hydrocarbon as eluent, or a mixture of such hydrocarbons, which allows a product of> 98% purity to be obtained with a yield of up to 95%. In the second stage, 1,2-di (methoxycarbonyl) benzo [gh] perylene obtained in the first stage, a mixture of molten succinonitrile with 1,2-dimethoxyethane in a volume ratio of 3: 1 to 1, is introduced into the reactor isolated from the access of light: 3, in an amount of 5 to 20 ml of this mixture per 1 mmol of 1,2-di (methoxycarbonyl) benzo [gh] perylene, and cesium fluoride in an amount of 2 to 8 mmol per 1 mmol of 1,2-di (methoxycarbonyl) benzo [ghi] perylene, then 2-trimethylsilylphenyl triflate is introduced into the reaction mixture in an amount of 2 to 8 mmol, per 1 mmol of 1,2-di (methoxycarbonyl) benzo [ghi] perylene, and then the contents of the reactor are stirred at a temperature of 40 to 100 ° C, in an inert gas atmosphere, for at least 12 hours, then, after completion of the gasoline cycloaddition reaction, the contents of the reactor are cooled to a temperature of not more than 50 ° C, and volatile fractions are evaporated, and the residue is washed several times with liquid saturated aliphatic hydrocarbon, then several times with water, after further purification by normal phase column chromatography is carried out, where the stationary phase is silica gel, the mobile phase is a mixture of saturated hydrocarbon liquid with methylene chloride in a volume ratio of 10: 1 to 1: 1, resulting in a product in the form of 1, 2-di (methoxycarbonyl) benzo [1,2-j] coronene with purity> 98% in yield up to 65%. |
| priorityDate | 2020-03-18-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| type | http://data.epo.org/linked-data/def/patent/Publication |
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