Preparation method of delta 16 steroid
The invention relates to a preparation method of a delta 16 steroid. At the atmosphere of protective gas, a compound of a formula II, an oxidizing agent and sulfur dioxide are subjected to a reaction in an organic solvent, the reaction temperature ranges from minus 50 DEG C to 0 DEG C, and the react...
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creator | XIE LONGYONG LIU XIRONG |
description | The invention relates to a preparation method of a delta 16 steroid. At the atmosphere of protective gas, a compound of a formula II, an oxidizing agent and sulfur dioxide are subjected to a reaction in an organic solvent, the reaction temperature ranges from minus 50 DEG C to 0 DEG C, and the reaction time is 1.5-2.5 h to obtain a delta 16 steroid I, wherein R1 is selected from H, halogen and acyloxy or hydroxide of C1-5; R2 is selected from alkyl of alpha C1-3 and alkyl or H of beta C1-2; R3 is selected from H, alkyl of alpha C1-3, alkyl of beta C1-2, alpha halogen or beta halogen; R4 and R5 are equal to H or double bonds; R7 is selected from H, and R6 is selected from H, alkyl of C1-3 or acyloxy of C1-5; or R6 and R7 are equal to double bonds. According to the preparation method of the delta 16 steroid, the 17-bit hydroxide compound of the formula II is used as raw materials, and the compound of the formula II is industrially produced and is easy to obtain; the preparation method is mild in reaction condition, no high-temperature strong base or strong acid is needed, fewer by-products are produced, the product yield and purity are high, the yield reaches more than 90%, and the purity reaches more than 93%. |
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At the atmosphere of protective gas, a compound of a formula II, an oxidizing agent and sulfur dioxide are subjected to a reaction in an organic solvent, the reaction temperature ranges from minus 50 DEG C to 0 DEG C, and the reaction time is 1.5-2.5 h to obtain a delta 16 steroid I, wherein R1 is selected from H, halogen and acyloxy or hydroxide of C1-5; R2 is selected from alkyl of alpha C1-3 and alkyl or H of beta C1-2; R3 is selected from H, alkyl of alpha C1-3, alkyl of beta C1-2, alpha halogen or beta halogen; R4 and R5 are equal to H or double bonds; R7 is selected from H, and R6 is selected from H, alkyl of C1-3 or acyloxy of C1-5; or R6 and R7 are equal to double bonds. According to the preparation method of the delta 16 steroid, the 17-bit hydroxide compound of the formula II is used as raw materials, and the compound of the formula II is industrially produced and is easy to obtain; the preparation method is mild in reaction condition, no high-temperature strong base or strong acid is needed, fewer by-products are produced, the product yield and purity are high, the yield reaches more than 90%, and the purity reaches more than 93%.</description><language>eng</language><subject>CHEMISTRY ; METALLURGY ; ORGANIC CHEMISTRY ; STEROIDS</subject><creationdate>2016</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=20160120&DB=EPODOC&CC=CN&NR=105254697A$$EHTML$$P50$$Gepo$$Hfree_for_read</linktohtml><link.rule.ids>230,308,780,885,25564,76547</link.rule.ids><linktorsrc>$$Uhttps://worldwide.espacenet.com/publicationDetails/biblio?FT=D&date=20160120&DB=EPODOC&CC=CN&NR=105254697A$$EView_record_in_European_Patent_Office$$FView_record_in_$$GEuropean_Patent_Office$$Hfree_for_read</linktorsrc></links><search><creatorcontrib>XIE LONGYONG</creatorcontrib><creatorcontrib>LIU XIRONG</creatorcontrib><title>Preparation method of delta 16 steroid</title><description>The invention relates to a preparation method of a delta 16 steroid. At the atmosphere of protective gas, a compound of a formula II, an oxidizing agent and sulfur dioxide are subjected to a reaction in an organic solvent, the reaction temperature ranges from minus 50 DEG C to 0 DEG C, and the reaction time is 1.5-2.5 h to obtain a delta 16 steroid I, wherein R1 is selected from H, halogen and acyloxy or hydroxide of C1-5; R2 is selected from alkyl of alpha C1-3 and alkyl or H of beta C1-2; R3 is selected from H, alkyl of alpha C1-3, alkyl of beta C1-2, alpha halogen or beta halogen; R4 and R5 are equal to H or double bonds; R7 is selected from H, and R6 is selected from H, alkyl of C1-3 or acyloxy of C1-5; or R6 and R7 are equal to double bonds. According to the preparation method of the delta 16 steroid, the 17-bit hydroxide compound of the formula II is used as raw materials, and the compound of the formula II is industrially produced and is easy to obtain; the preparation method is mild in reaction condition, no high-temperature strong base or strong acid is needed, fewer by-products are produced, the product yield and purity are high, the yield reaches more than 90%, and the purity reaches more than 93%.</description><subject>CHEMISTRY</subject><subject>METALLURGY</subject><subject>ORGANIC CHEMISTRY</subject><subject>STEROIDS</subject><fulltext>true</fulltext><rsrctype>patent</rsrctype><creationdate>2016</creationdate><recordtype>patent</recordtype><sourceid>EVB</sourceid><recordid>eNrjZFALKEotSCxKLMnMz1PITS3JyE9RyE9TSEnNKUlUMDRTKC5JLcrPTOFhYE1LzClO5YXS3AyKbq4hzh66qQX58anFBYnJqXmpJfHOfoYGpkamJmaW5o7GxKgBADkZJwE</recordid><startdate>20160120</startdate><enddate>20160120</enddate><creator>XIE LONGYONG</creator><creator>LIU XIRONG</creator><scope>EVB</scope></search><sort><creationdate>20160120</creationdate><title>Preparation method of delta 16 steroid</title><author>XIE LONGYONG ; LIU XIRONG</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-epo_espacenet_CN105254697A3</frbrgroupid><rsrctype>patents</rsrctype><prefilter>patents</prefilter><language>eng</language><creationdate>2016</creationdate><topic>CHEMISTRY</topic><topic>METALLURGY</topic><topic>ORGANIC CHEMISTRY</topic><topic>STEROIDS</topic><toplevel>online_resources</toplevel><creatorcontrib>XIE LONGYONG</creatorcontrib><creatorcontrib>LIU XIRONG</creatorcontrib><collection>esp@cenet</collection></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext_linktorsrc</fulltext></delivery><addata><au>XIE LONGYONG</au><au>LIU XIRONG</au><format>patent</format><genre>patent</genre><ristype>GEN</ristype><title>Preparation method of delta 16 steroid</title><date>2016-01-20</date><risdate>2016</risdate><abstract>The invention relates to a preparation method of a delta 16 steroid. At the atmosphere of protective gas, a compound of a formula II, an oxidizing agent and sulfur dioxide are subjected to a reaction in an organic solvent, the reaction temperature ranges from minus 50 DEG C to 0 DEG C, and the reaction time is 1.5-2.5 h to obtain a delta 16 steroid I, wherein R1 is selected from H, halogen and acyloxy or hydroxide of C1-5; R2 is selected from alkyl of alpha C1-3 and alkyl or H of beta C1-2; R3 is selected from H, alkyl of alpha C1-3, alkyl of beta C1-2, alpha halogen or beta halogen; R4 and R5 are equal to H or double bonds; R7 is selected from H, and R6 is selected from H, alkyl of C1-3 or acyloxy of C1-5; or R6 and R7 are equal to double bonds. According to the preparation method of the delta 16 steroid, the 17-bit hydroxide compound of the formula II is used as raw materials, and the compound of the formula II is industrially produced and is easy to obtain; the preparation method is mild in reaction condition, no high-temperature strong base or strong acid is needed, fewer by-products are produced, the product yield and purity are high, the yield reaches more than 90%, and the purity reaches more than 93%.</abstract><oa>free_for_read</oa></addata></record> |
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subjects | CHEMISTRY METALLURGY ORGANIC CHEMISTRY STEROIDS |
title | Preparation method of delta 16 steroid |
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