CS264016B1 - Způsob výroby N-oxadiethylenbenzoth5.azolyl-2-sulfonamidu - Google Patents

Způsob výroby N-oxadiethylenbenzoth5.azolyl-2-sulfonamidu Download PDF

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Publication number
CS264016B1
CS264016B1 CS843719A CS371984A CS264016B1 CS 264016 B1 CS264016 B1 CS 264016B1 CS 843719 A CS843719 A CS 843719A CS 371984 A CS371984 A CS 371984A CS 264016 B1 CS264016 B1 CS 264016B1
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CS
Czechoslovakia
Prior art keywords
preparation
morpholine
oxadiethylene
benzothiazol
sulfonamide
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Application number
CS843719A
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English (en)
Other versions
CS371984A1 (en
Inventor
Pavel A Pirogov
Raisa A Akcurina
Raisa S Levina
Boris N Gorbunov
Vladimir I Paramonov
Stanislav J Sizov
Vladimir G Skolnyj
Stanislav A Anosin
Nikolaj P Utrobin
Stanislav V Suchanov
Vjaceslav K Rykov
Original Assignee
Pavel A Pirogov
Raisa A Akcurina
Raisa S Levina
Boris N Gorbunov
Vladimir I Paramonov
Stanislav J Sizov
Vladimir G Skolnyj
Stanislav A Anosin
Nikolaj P Utrobin
Stanislav V Suchanov
Vjaceslav K Rykov
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Pavel A Pirogov, Raisa A Akcurina, Raisa S Levina, Boris N Gorbunov, Vladimir I Paramonov, Stanislav J Sizov, Vladimir G Skolnyj, Stanislav A Anosin, Nikolaj P Utrobin, Stanislav V Suchanov, Vjaceslav K Rykov filed Critical Pavel A Pirogov
Priority to CS843719A priority Critical patent/CS264016B1/cs
Publication of CS371984A1 publication Critical patent/CS371984A1/cs
Publication of CS264016B1 publication Critical patent/CS264016B1/cs

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Abstract

Způsob výroby N-oxadiethylenbenzothiazolyl-2-sulfenamidu spočívá ve vzájemném působení 2-merkaptobenzothiazolu s morfolinem, použitým v přebytku za přítomnosti peroxidu vodíku. Frooes probíhá za přidávání peroxidu vodíku v morfolinu k smési 2-merkaptobenzothiazolu a morfolinu.

Description

1 264016 ΟΠΗΟΑΗΗΕ Η3ΟΒΡΕΤΕΗΗΉ K ABTOPCKOMY CBHflETEJIbCTBY3aHBJieHo: 09.01.783anBKa Ν’ 2565916/23-04MKHZ C 07 D 277/80, C 08 I 3/24
Abtopm: Π,Α.Πηρογοβ, P.A.AicjypHHa, P.C.JIeBHHa, B.H.ropčyHOB, B.H.IIapaMOHOB,C.K),Ch30b, B.r.UlKonbHbiň, C.A.Ahoumh, Η.Π.ΥτροΒηη, C.B.CyxaHOB,B.K.Pmkob í 3aHBHTejib! aBTopbi .
Haasaime Η3θ6ρετβΗΗ«: OTOCOB nOJIY3EHHJI!N-OKCAflH3TEnEHBEH3THA30JfflJI-2-CyjIb-ΦΕΗΛΜΗβΑ. H3o6peTeHne othochtch k cnocoGy nonyqeHHH N-oKcaflH9THneH0eH3THa3anHJi-2- icynM>eHaMima (cyni4>eHaMHfla Μ) , κοτορΜή Hcno«b3yioT b XHMHnecKoň npoMumneHHoe-íth B xanecTBe ycKopHTena BynKaHHsartHH KayqyxoB 06mero HasHaqeHHH. ; H3BecTeH cnocoS nanyqeHHH cyjib$enaMHfla M, aaKnioqaraiiiHňcH b tom, ίτο CMecb J2-MepKanTo6eH3THa3ona vt ΜορφοπΗΗε noflBepraioT BgaHMoneňcŤBHio c οκκοπΗτεπεΜ brtjpHcyTCTBHH BOflbí £lj. B KanecTse OKHCJiHTeneft HcnoJibsyeTCH xuop, SpoM, ňoflηπη γηποχπορη« mejioHHoro: MeTanna. OKMCJieHHe προβοαητ npH TeMnepaType 25-40 C;B TeHeHHe 10-20 MHHyT. GOQTHODieHHe 2-ΜβρΚΒΠΤθ6βΗ3ΤΗ33ΟΠ í μορΦοπηη paBHO1:(8-10). Bbixoň 94-96%. T.nji. 85°C.
Cnoco6 xapaKTepH3yeTca Hcnonb3OBaHHeM b npouecce ranoreHa, TpyqHOCTHMHpereHepanHH η30μτοηηογο Μορφοπηκη BBuny nonyqeHHfl Ďaňbůůfó KOJiHnecTBa MHHe-panbHbix ccwieň, U6iibio M3o6peTeHHH HanaeTCfl ynpomeHHe τθχηοπογηη nonyneHHH cyju4*eHeMHAa Mh ynymneHne xanecTBa npoflyKTa. llocTaBJíeHHaa nenb flocTHraeTcn cnoco0OM, saKnioqaioiqHMcn b tom, ίτο CMecb2-MepKanTo6eH3THa3ona c μορΦοπηηομ o6pa6araBaioT nepeKHCbio BOflopoaa B Μορφο-jiHite.
Ecjih nepeKHCb BOflOpcwa «oĎaBjíHTb κ cMecH. 2-MepKanŤo0eH3Tna3ona η Μορφο-jiHHa 6e3 npemBapHTanbHoro cMenieHHH ee c μορΦοπηηομ, το neneeoň προηγκτ no·» - 2 - 264016 nynaeTcn c hh3khm BbixonoM (70%, T.nn. 83-84°C). IIpoBefleHHe peaKUHH nepe3npoflyKT B3anMOfleňcTBHH ΜορφοπΗΗβ c nepeKHCbio Boflopofla HCKnranaeT pa# noóon-Hbix peaKujíň, b pe3ynbTaTe uero noBbímaeTCH Bbixofl nponyKTa h ynynmaeTCfl eroKanecTBo (βμχοα 90-94%, T.nn. 86-87°C).
Jlnn npoBefleHHH peaKUHH 2-MepKanTo6eH3THa3on pacTBopnioT b ΜορφοπκΗε (co-OTHomeHHe 2-MepKanTo6eH3THa3on: μορΦοπηη 1:5,6) h floSaBJíaioT κ nonyneHHOMypacTBopy CMecb ΜορφαπΗΗβ h nepeKHCH Bonopona (cooTHomeHHe μορΦοπηη:nepeKHCbBOflopofla 1:(2,7-4) β TeneHHe 5-7 MHHyT, ΜορΦοπηη peraHepHpyioT c bhxqhom 95% Ha kqjiohhb c 3aTonneHHOH HacanKoňb τόκε yrjieKHcnoTbi, KOTopan nHpKynHpyeT b 33MKHyTOM utHicne. ΠρΗΜερ 1. B Tpexropnyio Kon6y εΜκοετωο 350 μπ, cHa6aceHHyio MenianKoň η τερΜΟΜετροΜ,3arpywaioT 20 r (0,12 γ-μοπ) 2-MepKanTO&eH3Tna3OJia h 60 μπ (0,68 γ-μοπ) Mop-φΟΠΗΗε, CMGCb Η3ΓρεΒ3Κ)Τ flO 60°C H BblflGpjKHBaiOT XipH 3TOÍI TGMnepaTypG 10 MHH.IlanyHGHHbiň pacTBop oxnaatflaioT no 20°C η noSaBnnioT CMecb 60 μπ (0,68 γ-μοπ)ΜορφοπΗΗ3 η 15 μπ (0,168 γ~μοπ) nepeKHCH Bonopo,n;a β TeneHHe 5 MHHyT. TeMne-paTypa b peaKHjiOHHofí CMecH noflHHMaeTcn no 75-80°C. IIonynatoT 28,4 r εγπκφεΗ-aMuna M (Bbixofl 94%, cnHTan Ha 2-MepKanTo6eH3THa3on) c T.nn, 87°C. flnn BbmeneHHn cyni^eHaMMna M hs μορΦοπηηοβογο pacTBOpa κ nocnenneMy β τε-qeiffle 10 MHHyT npn TeMnepaType 20-25°C πρΗβεΒππιοτ sony b KónHnecTse, paBHOMKonHnecTBy ΜορφοπΗΗε, κοτοροε ocTaeTcn b peaKnHOHHoft Macce nocne okohhhhhhpeaKUHH oKHcneHHH. IIpnyneHHyio cycneH3Hio οτΦηπβτροβμβηιοτ, npoMbroaioT no pH « = 9 h cyinaT npn t° = 50°C. ΠρΗΜβρ 2. B Tpexropnyro Kon6y, cnaSacenHyro MenianKoň η τερΜΟΜβτροΜ, 3arpyxcaroT 20 r(0,12 γ-μοπ) 2-MepKanTo6eH3Tna3ona h 60 μπ (0,68 γ-μοπ) ΜορφοπΗΗβ, CMecbHarpeBaioT no TeMnepaTypw 60°C h BbtfjepjKHBaioT npn stoh TeMnepaType 10 MHHyT.nonyqenHbiH pacTBop oxnaacnaroT no ,20°C η ηοδβΒΠπιοτ CMecb 40 μπ (0,456 γ/μοπ)ΜθρφθΠΗΗ3 Η 15 ΜΠ (0,168 Γ~ΜΟπ) nepeKHCH BOflOpOfla Β ΤεΠεΗΗΘ 7 MHHyT. Ilony-naioT 27,2 r ογπΒφ6Η3ΜΗη& M, (Bbixon 90%, cnHTan Ha 2-MepKanTo6eH3raa3on),T.nn. 86°C. IIpoflyKT Bb^ennioT, iok onncaHO b npHMepe 1.
HacToaiUHH cnocoč πο3Βοπηθτ οΦορμητβ nponecc b HenpepbiBHOM BapHaHTe, o6ec-nenHBaeT nonyneHHe neneBoro nponyKTa βμοοκογο KanecTBa 0e3 ηοποπΗΗτεπΒΗΟΗohhctkh (T.nn. 86-87°C).
. ΦΟΡΜΥΠΑ H30BPETEHHH
Cnocóó nonyneHHn N-oKcanH3THneH6eH3THa3onHn-2-cyn^eHaMnna B3anMoneňcTBH-fteM 2-MepKanTo6eH3THa3ona c μορΦοπηηομ, β3ητημ β η36ητκθ, β npHcyTcTBHH okhc-πΗτεππ, OTJiHHa»HHftca τβΜ, πτο, c nenbro ynpomenHn τθχηοπογηη ηynynmeHHH KanecTsa nponyKTa, b xanecTBe οκκοπΗτεπη Hcncnb3yioT nepeKHCb bo-ňopofla h nponecc BenyT nyTeM noBaBneHHn nepeKHCH Bonopona β μορΦοηηηθ κ CMe-ch 2-MepKanTo6eH3THa3ona η μορΦοπηϊιη. UCTOHHHKH ΗΗφορΜΗΙξΗΗ, npHHHTbie BO BHHM3HHe ΠρΗ 3KCnepTH3e: 1. ΠβτεΗτ CIHA ...3600398, κπ. 260-306, ony6n. 1971.
P E Φ E P A T
CnOCOB nOJIYHEHHH N-0KCAíai3WinEHBEH3THA30JBtlI-2-CyJII4>EHAMHflA
Cnoco6 nonyneHHH. Ν-0Κ03ηΗ3ΤΗΠβΗ6εΗ3ΤΗ330ΠΗΠ-2-0νΠΒφβΗ3ΜΗη3 3aKnionaeTCH BOB3aHMoneHCTBHH 2~MepKanTo6eH3THa3ona c μορΦοπηηομ, Β3ητημ β H36biTKe β npH-cyTcTBHH nepeKHCH Bonopona. nponecc προΒοηπτ πρη noČaBneHHH nepeKHCH BOflopo-na η ΜορφοπΗΗβ η CMecH 2-MepKanTo6eH3THa3ona η μορΦοπηιμ. - 3 - 264016 ΠρΗ3ΗδΗο Η3ο6ρβτβΗΗβΜ no pesynbTaTaM 3KcnepTH3bi, ocymecTBjíeHHOň FocynapcT-
BeaiWM ΚοΜΗτετοΜ CCCE no flenaM Η30θρβτβΗΗ& η οτκρωτΗβ, ,

Claims (1)

  1. 264016 - 4 - PŘEDMĚT VYNÁLEZU Způsob výroby N-oxadiethylenbenzothlazolyl^--sulfenamidu reakcí 2-merkaptobenzothlazolu s morfo-línem, použitým v přebytku, za přítomnosti okysličo-vadla, vyznačujíoí se tím, že jako okysllčovadlo sepoužívá peroxid vodíku a reakce se provádí přidávánímperoxidu vodíku v morfolinu do směsi 2-merkaptobenzo-thiazolu a morfolinu.
CS843719A 1984-05-18 1984-05-18 Způsob výroby N-oxadiethylenbenzoth5.azolyl-2-sulfonamidu CS264016B1 (cs)

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Application Number Priority Date Filing Date Title
CS843719A CS264016B1 (cs) 1984-05-18 1984-05-18 Způsob výroby N-oxadiethylenbenzoth5.azolyl-2-sulfonamidu

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Application Number Priority Date Filing Date Title
CS843719A CS264016B1 (cs) 1984-05-18 1984-05-18 Způsob výroby N-oxadiethylenbenzoth5.azolyl-2-sulfonamidu

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CS371984A1 CS371984A1 (en) 1987-03-12
CS264016B1 true CS264016B1 (cs) 1989-05-12

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