http://rdf.ncbi.nlm.nih.gov/pubchem/patent/RU-2705809-C2
Outgoing Links
| Predicate | Object |
|---|---|
| assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_c39bd4196e5950e3a8c053008ca1f588 |
| classificationCPCAdditional | http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/Y02P20-55 |
| classificationCPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07D209-54 |
| classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D209-54 |
| filingDate | 2016-06-23-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| grantDate | 2019-11-12-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| inventor | http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_f704b773d58b93259aea084c4aecaab7 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_5df54a0930bb157d3a51fa1d51b606e4 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_bbd92bf1cb04bfb24c311858bcf323f6 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_741e90729de882269437fe5577f4d0af |
| publicationDate | 2019-11-12-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| publicationNumber | RU-2705809-C2 |
| titleOfInvention | Method for obtaining chiral intermediate of ledipasvir |
| abstract | FIELD: chemistry.SUBSTANCE: invention relates to a method for synthesis of S-5-azaspiro [2,4] heptane-6-carboxylic acid, which is a chiral intermediate compound of ice precipitam. Method comprises the following steps: S1: ring closure reaction is carried out between 1,1-dihalomethyl methyl cyclopropane and ethyl ester of N-Boc-glycine in an alkaline medium to obtain compound A; S2: the compound A is saponified, the BOC protective group is removed to obtain 5-azaspiro[2,4]heptane-6-carboxylic acid in the form of a racemate; S3: 5-azaspiro[2,4]heptane-6-carboxylic acid in the form of a racemate is asymmetrically separated to obtain S-5-azaspiro[2,4]heptane-6-carboxylic acid; wherein specific operations of said asymmetric separation at step S3 are as follows: after addition of separating agent, 5-azaspiro[2,4]heptane-6-carboxylic acid is heated in form of racemate in the presence of organic acid and organic aldehyde at temperature of 40–120 °C for 4–10 hours; cooling to room temperature and adding an inert solvent with crystallisation; precipitating S-5-azaspiro[2,4]heptane-6-carboxylic acid and a separating agent in form of a solid phase; recovered solid phase in form of a salt is dissolved and after recrystallisation obtaining S-5-azaspiro[2,4]heptane-6-carboxylic acid; wherein said separating agent is L-tartaric acid; wherein said organic acid is any of glacial acetic acid, ortho-propionic acid or ethylacetic acid; said organic aldehyde is any of n-propionic aldehyde, n-butyraldehyde or salicylic aldehyde.EFFECT: method is characterized by high efficiency, simple synthesis, low cost of the product, ease of production and is applicable for large-scale industrial production.7 cl, 12 ex |
| priorityDate | 2016-06-17-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
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