http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-109796461-B
Outgoing Links
| Predicate | Object |
|---|---|
| classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D487-20 |
| filingDate | 2018-12-30-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| grantDate | 2020-09-25-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| publicationDate | 2020-09-25-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| publicationNumber | CN-109796461-B |
| titleOfInvention | Preparation process of tadalafil impurity I |
| abstract | The invention discloses a preparation process of tadalafil impurity I, which comprises the following stepsThe following steps: (1) mixing tadalafil, N-halogenated succinimide and a solvent in a reaction vessel, stirring at 20-50 ℃ for reaction, and tracking the reaction by TLC, wherein the solvent is one or a combination of tetrahydrofuran, water and glacial acetic acid; the N-halogenated succinimide is selected from one or a combination of more of N-chlorosuccinimide, N-bromosuccinimide and N-iodosuccinimide; (2) after the reaction is stopped, slowly adding alkali liquor into the reaction liquid until the pH value of the solution is more than or equal to 7, stirring for 20-60 min, decompressing and evaporating the organic solvent, extracting the residual aqueous solution by dichloromethane, and concentrating the extract liquid to obtain a crude product; (3) and (4) carrying out chromatographic separation or recrystallization on the crude product by using a silica gel column to obtain an impurity I. The preparation process has the advantages of easily obtained raw materials, mild reaction conditions and simple operation, and the obtained tadalafil impurity I has good purity and meets the requirements of pharmacopoeia. |
| priorityDate | 2018-12-30-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 39.