METHOD OF OBTAINING MIXTURES OF ORGANOSILICONE-OLIGOSULPHANES

METHOD OF OBTAINING MIXTURES OF ORGANOSILICONE-OLIGOSULPHANES

Preparation of a mixture of organosilicon oligosulfanes with a high fraction of disulfane comprises (1) reacting suspensions of finely-divided sodium with sulfur and optionally washing and drying the Na2Sx formed; and (2) reacting the Na2Sx with a triorganylsilyl(ar)alkyl halide. Preparation of a mi...

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Hauptverfasser: MICHEL RUDOLF, MUENZENBERG JOERG
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ACYCLIC OR CARBOCYCLIC COMPOUNDS
ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAININGELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN,SULFUR, SELENIUM OR TELLURIUM
CHEMISTRY
METALLURGY
ORGANIC CHEMISTRY
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creator MICHEL RUDOLF
MUENZENBERG JOERG
description Preparation of a mixture of organosilicon oligosulfanes with a high fraction of disulfane comprises (1) reacting suspensions of finely-divided sodium with sulfur and optionally washing and drying the Na2Sx formed; and (2) reacting the Na2Sx with a triorganylsilyl(ar)alkyl halide. Preparation of a mixture of organosilicon oligosulfanes of formula (I), with a high fraction of disulfane (IA), by a 2-stage reaction comprises: (1) reacting suspensions of finely-divided sodium with sulfur in amounts corresponding to the stoichiometric amounts for Na2Sx in an inert organic solvent under inert gas at over 98 degrees C and filtering and optionally washing and drying the Na2Sx formed; and (2) reacting the resultant Na2Sx, (partly) dissolved or suspended in an organic solvent, with a triorganylsilyl(ar)alkyl halide of formula (II) and isolating the resultant (I). Z-Alk-Sx-Alk-Z (I) Z-Alk-Hal (II) Z = a triorganylsilyl group of the formula -Si(R )2R , -SiR
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Preparation of a mixture of organosilicon oligosulfanes of formula (I), with a high fraction of disulfane (IA), by a 2-stage reaction comprises: (1) reacting suspensions of finely-divided sodium with sulfur in amounts corresponding to the stoichiometric amounts for Na2Sx in an inert organic solvent under inert gas at over 98 degrees C and filtering and optionally washing and drying the Na2Sx formed; and (2) reacting the resultant Na2Sx, (partly) dissolved or suspended in an organic solvent, with a triorganylsilyl(ar)alkyl halide of formula (II) and isolating the resultant (I). Z-Alk-Sx-Alk-Z (I) Z-Alk-Hal (II) Z = a triorganylsilyl group of the formula -Si(R )2R , -SiR&lt;1)&lt;R )2 or -Si(R )3; R = 1-6C alkyl, 5-8C cycloalkyl, benzyl or a phenyl group, optionally substituted by (m)ethyl or chlorine; R = 1-6 C alkoxy,. 5-8 C cycloalkoxy, phenoxy or benzyloxy; Alk = a divalent, saturated, 1-10C hydrocarbon group or an aralkylene group of formula (III); n = 1-4; x = 1.5-3.0; and Hal = Cl or Br.</description><edition>6</edition><language>eng</language><subject>ACYCLIC OR CARBOCYCLIC COMPOUNDS ; ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAININGELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN,SULFUR, SELENIUM OR TELLURIUM ; CHEMISTRY ; METALLURGY ; ORGANIC CHEMISTRY</subject><creationdate>1999</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=19991108&amp;DB=EPODOC&amp;CC=PL&amp;NR=332850A1$$EHTML$$P50$$Gepo$$Hfree_for_read</linktohtml><link.rule.ids>230,308,780,885,25564,76547</link.rule.ids><linktorsrc>$$Uhttps://worldwide.espacenet.com/publicationDetails/biblio?FT=D&amp;date=19991108&amp;DB=EPODOC&amp;CC=PL&amp;NR=332850A1$$EView_record_in_European_Patent_Office$$FView_record_in_$$GEuropean_Patent_Office$$Hfree_for_read</linktorsrc></links><search><creatorcontrib>MICHEL RUDOLF</creatorcontrib><creatorcontrib>MUENZENBERG JOERG</creatorcontrib><title>METHOD OF OBTAINING MIXTURES OF ORGANOSILICONE-OLIGOSULPHANES</title><description>Preparation of a mixture of organosilicon oligosulfanes with a high fraction of disulfane comprises (1) reacting suspensions of finely-divided sodium with sulfur and optionally washing and drying the Na2Sx formed; and (2) reacting the Na2Sx with a triorganylsilyl(ar)alkyl halide. Preparation of a mixture of organosilicon oligosulfanes of formula (I), with a high fraction of disulfane (IA), by a 2-stage reaction comprises: (1) reacting suspensions of finely-divided sodium with sulfur in amounts corresponding to the stoichiometric amounts for Na2Sx in an inert organic solvent under inert gas at over 98 degrees C and filtering and optionally washing and drying the Na2Sx formed; and (2) reacting the resultant Na2Sx, (partly) dissolved or suspended in an organic solvent, with a triorganylsilyl(ar)alkyl halide of formula (II) and isolating the resultant (I). 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Preparation of a mixture of organosilicon oligosulfanes of formula (I), with a high fraction of disulfane (IA), by a 2-stage reaction comprises: (1) reacting suspensions of finely-divided sodium with sulfur in amounts corresponding to the stoichiometric amounts for Na2Sx in an inert organic solvent under inert gas at over 98 degrees C and filtering and optionally washing and drying the Na2Sx formed; and (2) reacting the resultant Na2Sx, (partly) dissolved or suspended in an organic solvent, with a triorganylsilyl(ar)alkyl halide of formula (II) and isolating the resultant (I). Z-Alk-Sx-Alk-Z (I) Z-Alk-Hal (II) Z = a triorganylsilyl group of the formula -Si(R )2R , -SiR&lt;1)&lt;R )2 or -Si(R )3; R = 1-6C alkyl, 5-8C cycloalkyl, benzyl or a phenyl group, optionally substituted by (m)ethyl or chlorine; R = 1-6 C alkoxy,. 5-8 C cycloalkoxy, phenoxy or benzyloxy; Alk = a divalent, saturated, 1-10C hydrocarbon group or an aralkylene group of formula (III); n = 1-4; x = 1.5-3.0; and Hal = Cl or Br.</abstract><edition>6</edition><oa>free_for_read</oa></addata></record>
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subjects ACYCLIC OR CARBOCYCLIC COMPOUNDS
ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAININGELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN,SULFUR, SELENIUM OR TELLURIUM
CHEMISTRY
METALLURGY
ORGANIC CHEMISTRY
title METHOD OF OBTAINING MIXTURES OF ORGANOSILICONE-OLIGOSULPHANES
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