http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-105503714-A
Outgoing Links
Predicate | Object |
---|---|
assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_cbd6afe8bf92cebfc1a738927809ab36 |
classificationCPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07D213-81 |
classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D213-81 |
filingDate | 2015-12-24-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
inventor | http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_8c7ed8b6fc7001101bff015f880b7b92 |
publicationDate | 2016-04-20-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationNumber | CN-105503714-A |
titleOfInvention | Synthesis method of piperidine carboxylic acid amide drug intermediate N-(2,6-dimethyl benzene)-4-pyridine carboxamide |
abstract | A synthesis method of piperidine carboxylic acid amide drug intermediate N-(2,6-dimethyl benzene)-4-pyridine carboxamide comprises steps as follows: 1.1 mol of pyridine-4-formamide and 600-620 ml of nitromethane are added to a reaction container provided with a stirrer and a thermometer, the stirring speed is controlled to range from 130 rpm to 160 rpm, 0.4-0.42 mol of cuprous bromide is added in batches, the temperature of the solution is increased to 100-105 DEG C, the solution reacts for 2-3 h, filtration is performed, a filtrate is added to the reaction container again, 1.1-1.3 mol of 2,6-xylidine is added dropwise, the stirring speed is kept for 5-6 h after addition, the temperature of the solution is decreased to 15-18 DEG C, solids separate out, filtration is performed, the solids are washed with ethyl acetate, N-(2,6-dimethyl benzene)-4-pyridine carboxamide bromate is obtained and dissolved in 1,100 ml of a potassium nitrate solution, decolorization is performed with a molecular sieve, a sodium sulfite solution is added to adjust the pH to range from 9 to 10, the temperature of the solution is decreased to 3-5 DEG C, solids separate out, filtration is performed, the solids are washed with a salt solution, dehydrated with a dehydrating agent and recrystallized in chlorobenzene, and the N-(2,6-dimethyl benzene)-4-pyridine carboxamide is obtained. |
priorityDate | 2015-12-24-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 48.