Method for removing impurities from palbociclib intermediate
The invention relates to a method for removing impurities from a palbociclib intermediate, and belongs to the technical field of medical chemistry. Methanol and water are used as refining solvents, activated carbon is added, heat preservation and stirring are performed, then methanol is removed thro...
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| creator | LIN QUANSHENG YANG BO REN CHUANDONG |
| description | The invention relates to a method for removing impurities from a palbociclib intermediate, and belongs to the technical field of medical chemistry. Methanol and water are used as refining solvents, activated carbon is added, heat preservation and stirring are performed, then methanol is removed through evaporation, and 4-(6-aminopyridine-3-yl) piperazine-1-carboxylic acid tert-butyl ester is obtained through filtering and drying. According to the refining method disclosed by the invention, azo impurities in the 4-(6-aminopyridine-3-yl) piperazine-1-carboxylic acid tert-butyl ester crude product can be effectively removed, a solid which is off-white or bright yellow in appearance is obtained, and the purity of the product reaches 99.9% or above.
本发明涉及一种哌柏西利中间体杂质的去除方法，属于医药化学的技术领域。本发明利用甲醇和水作为精制溶剂，加入活性炭保温搅拌后，蒸除甲醇，过滤干燥得4-(6-氨基吡啶-3-基)哌嗪-1-羧酸叔丁酯。通过本发明的精制方法，可以有效地将4-(6-氨基吡啶-3-基)哌嗪-1-羧酸叔丁酯粗品中的偶氮杂质去除，获得外观呈类白色或亮黄色的固体，产品的纯度达到99.9％以上。 |
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本发明涉及一种哌柏西利中间体杂质的去除方法，属于医药化学的技术领域。本发明利用甲醇和水作为精制溶剂，加入活性炭保温搅拌后，蒸除甲醇，过滤干燥得4-(6-氨基吡啶-3-基)哌嗪-1-羧酸叔丁酯。通过本发明的精制方法，可以有效地将4-(6-氨基吡啶-3-基)哌嗪-1-羧酸叔丁酯粗品中的偶氮杂质去除，获得外观呈类白色或亮黄色的固体，产品的纯度达到99.9％以上。</description><language>chi ; eng</language><subject>CHEMISTRY ; HETEROCYCLIC COMPOUNDS ; METALLURGY ; ORGANIC CHEMISTRY</subject><creationdate>2021</creationdate><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://worldwide.espacenet.com/publicationDetails/biblio?FT=D&date=20210430&DB=EPODOC&CC=CN&NR=112724078A$$EHTML$$P50$$Gepo$$Hfree_for_read</linktohtml><link.rule.ids>230,308,776,881,25542,76290</link.rule.ids><linktorsrc>$$Uhttps://worldwide.espacenet.com/publicationDetails/biblio?FT=D&date=20210430&DB=EPODOC&CC=CN&NR=112724078A$$EView_record_in_European_Patent_Office$$FView_record_in_$$GEuropean_Patent_Office$$Hfree_for_read</linktorsrc></links><search><creatorcontrib>LIN QUANSHENG</creatorcontrib><creatorcontrib>YANG BO</creatorcontrib><creatorcontrib>REN CHUANDONG</creatorcontrib><title>Method for removing impurities from palbociclib intermediate</title><description>The invention relates to a method for removing impurities from a palbociclib intermediate, and belongs to the technical field of medical chemistry. Methanol and water are used as refining solvents, activated carbon is added, heat preservation and stirring are performed, then methanol is removed through evaporation, and 4-(6-aminopyridine-3-yl) piperazine-1-carboxylic acid tert-butyl ester is obtained through filtering and drying. According to the refining method disclosed by the invention, azo impurities in the 4-(6-aminopyridine-3-yl) piperazine-1-carboxylic acid tert-butyl ester crude product can be effectively removed, a solid which is off-white or bright yellow in appearance is obtained, and the purity of the product reaches 99.9% or above.
本发明涉及一种哌柏西利中间体杂质的去除方法，属于医药化学的技术领域。本发明利用甲醇和水作为精制溶剂，加入活性炭保温搅拌后，蒸除甲醇，过滤干燥得4-(6-氨基吡啶-3-基)哌嗪-1-羧酸叔丁酯。通过本发明的精制方法，可以有效地将4-(6-氨基吡啶-3-基)哌嗪-1-羧酸叔丁酯粗品中的偶氮杂质去除，获得外观呈类白色或亮黄色的固体，产品的纯度达到99.9％以上。</description><subject>CHEMISTRY</subject><subject>HETEROCYCLIC COMPOUNDS</subject><subject>METALLURGY</subject><subject>ORGANIC CHEMISTRY</subject><fulltext>true</fulltext><rsrctype>patent</rsrctype><creationdate>2021</creationdate><recordtype>patent</recordtype><sourceid>EVB</sourceid><recordid>eNrjZLDxTS3JyE9RSMsvUihKzc0vy8xLV8jMLSgtyizJTC1WSCvKz1UoSMxJyk_OTM7JTFLIzCtJLcpNTclMLEnlYWBNS8wpTuWF0twMim6uIc4euqkF-fGpxQWJyal5qSXxzn6GhkbmRiYG5haOxsSoAQAmZzBg</recordid><startdate>20210430</startdate><enddate>20210430</enddate><creator>LIN QUANSHENG</creator><creator>YANG BO</creator><creator>REN CHUANDONG</creator><scope>EVB</scope></search><sort><creationdate>20210430</creationdate><title>Method for removing impurities from palbociclib intermediate</title><author>LIN QUANSHENG ; YANG BO ; REN CHUANDONG</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-epo_espacenet_CN112724078A3</frbrgroupid><rsrctype>patents</rsrctype><prefilter>patents</prefilter><language>chi ; eng</language><creationdate>2021</creationdate><topic>CHEMISTRY</topic><topic>HETEROCYCLIC COMPOUNDS</topic><topic>METALLURGY</topic><topic>ORGANIC CHEMISTRY</topic><toplevel>online_resources</toplevel><creatorcontrib>LIN QUANSHENG</creatorcontrib><creatorcontrib>YANG BO</creatorcontrib><creatorcontrib>REN CHUANDONG</creatorcontrib><collection>esp@cenet</collection></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext_linktorsrc</fulltext></delivery><addata><au>LIN QUANSHENG</au><au>YANG BO</au><au>REN CHUANDONG</au><format>patent</format><genre>patent</genre><ristype>GEN</ristype><title>Method for removing impurities from palbociclib intermediate</title><date>2021-04-30</date><risdate>2021</risdate><abstract>The invention relates to a method for removing impurities from a palbociclib intermediate, and belongs to the technical field of medical chemistry. Methanol and water are used as refining solvents, activated carbon is added, heat preservation and stirring are performed, then methanol is removed through evaporation, and 4-(6-aminopyridine-3-yl) piperazine-1-carboxylic acid tert-butyl ester is obtained through filtering and drying. According to the refining method disclosed by the invention, azo impurities in the 4-(6-aminopyridine-3-yl) piperazine-1-carboxylic acid tert-butyl ester crude product can be effectively removed, a solid which is off-white or bright yellow in appearance is obtained, and the purity of the product reaches 99.9% or above.
本发明涉及一种哌柏西利中间体杂质的去除方法，属于医药化学的技术领域。本发明利用甲醇和水作为精制溶剂，加入活性炭保温搅拌后，蒸除甲醇，过滤干燥得4-(6-氨基吡啶-3-基)哌嗪-1-羧酸叔丁酯。通过本发明的精制方法，可以有效地将4-(6-氨基吡啶-3-基)哌嗪-1-羧酸叔丁酯粗品中的偶氮杂质去除，获得外观呈类白色或亮黄色的固体，产品的纯度达到99.9％以上。</abstract><oa>free_for_read</oa></addata></record> |
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| title | Method for removing impurities from palbociclib intermediate |
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