Preparation method for crystalline dibenzothiazepine derivative

The invention discloses a preparation method for a crystalline dibenzothiazepine derivative. The crystalline dibenzothiazepine derivative is synthesized through chlorination reaction, condensation reaction and salt forming reaction by taking dibenzo[b,f][1,4]thiazepine-11-[10H]one as an initial raw...

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Hauptverfasser: GU ZHIYONG, CHI XIAONA, GUO PEI, LYU YAJUN, YANG HAOJIE, XU ANNA
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creator GU ZHIYONG
CHI XIAONA
GUO PEI
LYU YAJUN
YANG HAOJIE
XU ANNA
description The invention discloses a preparation method for a crystalline dibenzothiazepine derivative. The crystalline dibenzothiazepine derivative is synthesized through chlorination reaction, condensation reaction and salt forming reaction by taking dibenzo[b,f][1,4]thiazepine-11-[10H]one as an initial raw material. According to the preparation method, in preparation of 11-chlorine-dibenzo[b,f][1,4]thiazepine, phosphorus oxychloride which is high in toxicity and pollution is replaced by oxalyl chloride which is low in toxicity and pollution; the use of N,N-dimethyl aniline which is high in pollution is prevented, so that the pollution on the environment is greatly reduced; by virtue of salification by crystalline 11-[4-[2-(2-hydroxyl ethoxyl)ethyl]-1-piperazinyl]dibenzo[b,f][1,4]thiazepine free alkali, acquisition of high quality fumarate is ensured, the production cost is effectively lowered, and the batch production is facilitated.
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The crystalline dibenzothiazepine derivative is synthesized through chlorination reaction, condensation reaction and salt forming reaction by taking dibenzo[b,f][1,4]thiazepine-11-[10H]one as an initial raw material. According to the preparation method, in preparation of 11-chlorine-dibenzo[b,f][1,4]thiazepine, phosphorus oxychloride which is high in toxicity and pollution is replaced by oxalyl chloride which is low in toxicity and pollution; the use of N,N-dimethyl aniline which is high in pollution is prevented, so that the pollution on the environment is greatly reduced; by virtue of salification by crystalline 11-[4-[2-(2-hydroxyl ethoxyl)ethyl]-1-piperazinyl]dibenzo[b,f][1,4]thiazepine free alkali, acquisition of high quality fumarate is ensured, the production cost is effectively lowered, and the batch production is facilitated.</description><language>eng</language><subject>ACYCLIC OR CARBOCYCLIC COMPOUNDS ; APPARATUS THEREFOR ; CHEMISTRY ; GENERAL METHODS OF ORGANIC CHEMISTRY ; HETEROCYCLIC COMPOUNDS ; METALLURGY ; ORGANIC CHEMISTRY</subject><creationdate>2015</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&amp;date=20151125&amp;DB=EPODOC&amp;CC=CN&amp;NR=105085435A$$EHTML$$P50$$Gepo$$Hfree_for_read</linktohtml><link.rule.ids>230,308,776,881,25543,76293</link.rule.ids><linktorsrc>$$Uhttps://worldwide.espacenet.com/publicationDetails/biblio?FT=D&amp;date=20151125&amp;DB=EPODOC&amp;CC=CN&amp;NR=105085435A$$EView_record_in_European_Patent_Office$$FView_record_in_$$GEuropean_Patent_Office$$Hfree_for_read</linktorsrc></links><search><creatorcontrib>GU ZHIYONG</creatorcontrib><creatorcontrib>CHI XIAONA</creatorcontrib><creatorcontrib>GUO PEI</creatorcontrib><creatorcontrib>LYU YAJUN</creatorcontrib><creatorcontrib>YANG HAOJIE</creatorcontrib><creatorcontrib>XU ANNA</creatorcontrib><title>Preparation method for crystalline dibenzothiazepine derivative</title><description>The invention discloses a preparation method for a crystalline dibenzothiazepine derivative. 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The crystalline dibenzothiazepine derivative is synthesized through chlorination reaction, condensation reaction and salt forming reaction by taking dibenzo[b,f][1,4]thiazepine-11-[10H]one as an initial raw material. According to the preparation method, in preparation of 11-chlorine-dibenzo[b,f][1,4]thiazepine, phosphorus oxychloride which is high in toxicity and pollution is replaced by oxalyl chloride which is low in toxicity and pollution; the use of N,N-dimethyl aniline which is high in pollution is prevented, so that the pollution on the environment is greatly reduced; by virtue of salification by crystalline 11-[4-[2-(2-hydroxyl ethoxyl)ethyl]-1-piperazinyl]dibenzo[b,f][1,4]thiazepine free alkali, acquisition of high quality fumarate is ensured, the production cost is effectively lowered, and the batch production is facilitated.</abstract><oa>free_for_read</oa></addata></record>
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subjects ACYCLIC OR CARBOCYCLIC COMPOUNDS
APPARATUS THEREFOR
CHEMISTRY
GENERAL METHODS OF ORGANIC CHEMISTRY
HETEROCYCLIC COMPOUNDS
METALLURGY
ORGANIC CHEMISTRY
title Preparation method for crystalline dibenzothiazepine derivative
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