CS260013B1 - Způsob výroby ftalimidů alkalických kovů - Google Patents
Způsob výroby ftalimidů alkalických kovů Download PDFInfo
- Publication number
- CS260013B1 CS260013B1 CS843729A CS372984A CS260013B1 CS 260013 B1 CS260013 B1 CS 260013B1 CS 843729 A CS843729 A CS 843729A CS 372984 A CS372984 A CS 372984A CS 260013 B1 CS260013 B1 CS 260013B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- phthalimides
- pactbopa
- πρκ
- production
- alcoholic
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract 3
- 125000005543 phthalimide group Chemical class 0.000 title claims abstract 3
- 229910052751 metal Inorganic materials 0.000 title abstract 2
- 239000002184 metal Substances 0.000 title abstract 2
- 150000002739 metals Chemical class 0.000 title abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract 4
- 230000001476 alcoholic effect Effects 0.000 claims abstract 4
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract 2
- -1 alkali metal alkoxide Chemical class 0.000 claims abstract 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000003513 alkali Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 230000003993 interaction Effects 0.000 abstract 1
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 abstract 1
- 235000009421 Myristica fragrans Nutrition 0.000 description 7
- 239000001115 mace Substances 0.000 description 7
- QXOQNNAWFUXKMH-UHFFFAOYSA-N 1-(Malonylamino)cyclopropanecarboxylic acid Chemical compound OC(=O)CC(=O)NC1(C(O)=O)CC1 QXOQNNAWFUXKMH-UHFFFAOYSA-N 0.000 description 2
- UGTJLJZQQFGTJD-UHFFFAOYSA-N Carbonylcyanide-3-chlorophenylhydrazone Chemical compound ClC1=CC=CC(NN=C(C#N)C#N)=C1 UGTJLJZQQFGTJD-UHFFFAOYSA-N 0.000 description 2
- 101150104923 CPOX gene Proteins 0.000 description 1
- 240000006890 Erythroxylum coca Species 0.000 description 1
- 101100066898 Mus musculus Flna gene Proteins 0.000 description 1
- 241000549556 Nanos Species 0.000 description 1
- 101100184172 Schizosaccharomyces pombe (strain 972 / ATCC 24843) mkh1 gene Proteins 0.000 description 1
- JKKPSTXVKNWEAH-VWHZSNQBSA-N bbip Chemical compound NC(=N)NCCC[C@@H](C(N)=O)NC(=O)[C@H](C(C)C)NC(=O)[C@H](CCCNC(N)=N)NC(=O)[C@H](CCCNC(N)=N)NC(=O)[C@H](CC(C)C)NC(=O)[C@@H]1CCCN1C(=O)[C@H]1N(C(=O)[C@H](CCCNC(N)=N)NC(=O)[C@H](CCCCN)NC(=O)[C@H](CC=2C=CC=CC=2)NC(=O)[C@H](CCCCN)NC(=O)CNC(=O)C=2C=CC(=CC=2)C(=O)C=2C=CC=CC=2)CCC1 JKKPSTXVKNWEAH-VWHZSNQBSA-N 0.000 description 1
- 235000008957 cocaer Nutrition 0.000 description 1
- ZPUCINDJVBIVPJ-LJISPDSOSA-N cocaine Chemical compound O([C@H]1C[C@@H]2CC[C@@H](N2C)[C@H]1C(=O)OC)C(=O)C1=CC=CC=C1 ZPUCINDJVBIVPJ-LJISPDSOSA-N 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Způsob výroby ftalimidů alkalických
kovů spočívá ve vzájemném působení ftalimidu
s alkoholickým roztokem hydroxidu
a/nebo alkoholátem alkalického kovu ve vakuu
při teplotě 50 až 140 °C. Páry alkoholu
a vogy, které při reakci yznikaií, ae.odstraňují
rychlostí, zajištující v reakční
hmotě pro přívod alkoholiokeho roztoku koncentraci
alkoholu 10 až 60 % hmot.
Description
-1- OIIHCAHHE Μ30ΒΡΕΤΕΗΗΉ K ABTOPCKOMY CBHHETEJIBCTBY3aHBneHo·. 01.03.823a«BKa: »3401628/23-04 MKH1 C 07 D 209/48
Abtoph: Α.Α.Οβηηηηηκοβ, Β.Π.Αυηηη, Β,Β.Κοποβ, Β.Η.Χπη6οβ, KhM.PanonopT, Β.Η.ΓορδγΗΟΒ, Ε.C.MaKapoBa, B.B.flaBHTynHaHH, C.H.3aňpeBa
3anBHTenb:HayMHO-HccnenoBaTejibCKHň ηηοτητυτ χημηκβτοβ ηπη nonHMepHbix Μβτβ-pnajioB
HaaeaHHe Η3θόρβτβΗΗΗί CnOCOB ΠΟΛΠΕΗΗΗ ΦΤΑΠΗΜΗβΟΒ IHEJIOHHMX METAJ1JI0B Η3θ6ρβΤβΗΗβ OTHOCHTCfl K CnOCOĎy nOJiyueHHH φΤβΠΗΜΗβΟΒ mejIOHHblX ΜβΤ3ΠΠΟΒ,ncnojib3yeMbix b xanecTBe npoMexyroqHwx προμγκτοΒ npH cHHTese 3aMennHTeneňnoflByjiKaHHaauHH KaynyKOB. IÍ3BecTeH cnocoS noJiyxeHHH φταπΗΜΗ/χβ xanHA BsáHMOfteftcTBHeM 5%-ηογο pacTBO-pa φΤΗΠΗΜΗβΒ B a6cOJDOTHOM STaHOJie C 25%“HbIM 3TaH0JlbHbIM paCTBOpOM rHflpOKCHflaKaJiHH (1). Ilocne cjihbhhhh pacTBOpoB peaKUHOHHyro Maccy Shctpo oxnaxnaioT, ot-φΗΠΐ>τροΒΗΒέιοτ Φτηπημηχχ KaJiHH, ocaflOK cycneHflHpyroT b aueTOHe, φκπΒτργιοτ h cy-maT npH yMepeHHOM HarpeBe Ha Bosnyxe. Bmxojx nponyxTa cocTaBnaeT οκοπο 90%.
Cnoco6 xapaxTepHayeTCH h6bhcokhm βηχοπομ xxeneBoro npojxyKTa, 3HanHTenbHbiMpaCXOflOM 3T3HOJI3 Η aiXeTOHa, BapMBO- H nOXapOOnaCHOCTbIO HCnOJIbSyeMblX paCTBO-pHTejieň.
HaBecTeH Taxxe cnócoC nonyHeHHfl Φτηπημηχχοβ mejioHHbix MeTannoB B3aHMOfleňcT-ΒΗΘΜ eyeneHSHH ΤΟΗΚΟΗ3ΜβήΒΗβΗΗΟΓΟ φΤ8ΠΗΜΗΑ3 B ΟββΒΒΟΧβΗΗΜΧ βΠΗφβΤΗ’ϊβΟΚΗΧcnnpTax, coflep»amnx b MOJiexyne οτ 1 no 4 aTOMOB yrnepona, c paČTBopoM riw-poKCHfta ηπη anKorojiHTa menoHHoro MeTanna b Tex xe cnHpTax (2). Ilpoixecc npo-BoflHŤ npn 35-.5Ó°C b TeneHHe 1-6 ňacos. Ilocne BHflepXKH cycneH3Hio oxnaxxxaioTno 20°C, ocaflOK npoMbisa»T οπκρτοΜ h cyraaT, Bbjxojx xxeneBoro npojxyKTa cocTaB-πηθτ 85%.
Cnocoó xapaKTepH3yeTCH hhskhm buxoxxom xxeneBoro nponyKTa. 260013 -2-
HaH6oJiee 6πη3κημ k Η9θ6ρετβΗΗΐο no TexHunecKóň cyiRHOCTH h flocraraeMOMypeayjibTaTy HBJíaeTCH cnocoč nonyneHHH φτβηηΜΗηοΒ menonHbix MeTannoB, 3aKJiio-nawmHňcH b tom, hto b cycneH3wo irrajiHMnpa b oprammecKOM pacTBopuTene npnTeMnepaType 50-110°C b Tenemie 60-70 MHi^yT p,o3npyioT cMecb pacTBópoB ČyTHJiaTamenonHoro MeTanna n runpoKCHna menonHoro MeTanna b opramojecKOM pacTBopuTe-Jie npH MOnbHOM ^COOTHOineHHH, paBHOM 0,5:0,5-0,99:0,01 COOTBeTCTBeHHO. CHHTC3npoBOflHT b eMKOCTHoM annapaTe, cHa6weHHOM MeinajiKoň h oBpaTHWM χοβοαιπιβηηκομfljia BO3BpaTa napoB pacTBopHTejia. ílocne ποβηογο CMeineHna peareHTOB peaKitfioH-Hyio Maccy BbfflepjKHBawT 20 MHHyT, oxnaatnaioT, (JmjibTpyroT h BbicyuiHBaroT. flnn npn-roTOBJíeHHH cycneH3HH (J>TajiHMHfla b xanecTBe opramreecKoro pacTBopuTejin hc-nojib3yioT 6yTaHoji, 6eH3OJi, xjiop6eH3OJi, yaňT-cnHpT. Bbixofl nponyKTa cocTaBJíneT97-992!, coflepxaHne ocHOBHoro eemecTBa - 95-99% (3).
Cnoeo6 ΗΜβετ cnowHbie h nnHTenbHbie BcnoMoraTenbHbte cTanHH φκηΒτροΒΒΗΗΗ hcymKH npoflyKTa ot opraHHnecKoro pacTBopHTenn. CycneH3HR nponyKTa, nonyneH-ηογο yKa3aHHbiM cnocoSoM, HeynoBneTBopHTenbHo φΗηΒτργθτοΗ, ocanoK πηοχο ot-jKHMaeTca h cop,ep)KHT 3HannTenbHoe KOJinnecTBO (20-30% Mace.) pacTBopHTenn. Ot-φΚΠΒΤρθΒ3ΗΗ3Β naCTa CKJIOHHa K THKCOTponHOMy pa3JIO»ceHHK) npn BO3fleňCTBHH Me-xaHHnecKHX BO3n,eňcTBHň, HannnaeT Ha MeTannHnecKHe noBepxHocTH, hto cymecT- BeHHo ycnowHReT TpaHcnopTHpOBKy nacTbi οτ φκηΒτρβ κ cymHJiKe. HanHnaHHe npo-nyKTa Ha οτθηκη η ροτορ BaKyyM-rpeĎKOBoft cynimiKH 3aTpynHneT nponecc cyniKH,flenaeT ero ηππτεηΒΗΜΜ η ΜβποοφφβκτΗΒΗωΜ. flnHTenbHocTb cymKH cocTaBnaeT 5-6 nacoB, Bcero nponecca - 6,5-8,5 MacoB. < Iíejib HacTOHmero Η3θ6ρβτβΗΗ« 3aKnioyajÍacb ·β ynpomeHHH η ΗΗΤθΗΟΗφΗΚβηΗΗ.nponecca. IIocTaBJíeHHaR nenb nocTHraeTCH cnocoČOM nonyneHHH φτβηΗΜΗηοε menoHHbix Μβ-TannOB nyTeM B3aHMOneftCTBHH φΤβΗΗΜΗΛβ CO CnHpTOBblM paCTBOpOM rHfípOKCHflah/hjih ajiKoroJiHToM menoHHoro MeTanna npn TeMnepaType 50-140°C, oTJiHHaromjjňcHτθμ, hto BsaHMOfleňcTBHe BenyT non BaKýyMOM h BbwenmomHecn napw cnHpTa h bo-flbí yflanHioT co CKopocTbio, oCecnenHBaiomeň b peaKUHOHHoň Macce b nponecce no-flanH cnnpTOBoro pacTBopa KoHneHTpanHio cnHpTa 10-60% Mace.
CornacHo ffaHHOMy cnoco6y cHHTe3 φτβηΗΜκηοΒ menoHHbix ΜβτεηηοΒ προΒορ,ΗΤ b-CMecHTejiHX, npHcnoco6jieHHbix nnn πθρθμθπιηββηηη nacToo6pa3Hbix nponyKTOB,HanpHMep, b CMecHTenHX Tuna ΒβρΗβρ-ΠφπβΗηβρβρ. nponecc προΒοηητ npH TeMne-paType 50-140°C, npennoHTHTenbHo πρκ TeMnepaType 70-80°C. Πρκ τθμπθ-j paType nponecca Bbnne 140°C cymecTseHHo CHuacaeTcn conepacaHHe ochob-ηογο BemecTBa b yeneBOM προηγκτε, πρκ TeMnepaType MeHee 50°C yBe·?nHHHBaeTCB npoflOjDKHTejibHocTb nponecca h cHHxaeTCH KanecTBO nponyK-Ta. B xanecTBe opraHHuecKoro pacTBopHTenn ajih πρηγοτοβπθηηη pacTBopa γηαροκ-CHfla ηπη anKorojwTa menonHoro MeTanna HCnonb3yioT ajmfcaTHHecKHe οπκρτΜ, co-flepxamne 1-4 aTOMa yrnepona b Monenyne. CnHpTOBbiň pacTBop πρκ nepeMeuiHBaHHHnocTeneHHo nonaioT b CMecnTenb Ha npeflBapHTenbHO HarpeTbiň no 50-100°C φτβηκ-MHfl. Ilapbl cnHpTa H BOflbl, BbffleJIH!OmeftCH B npOIjeCCe B3aHMOReňCTBHH, ynajIHIOT H33OHbi peaKHHH, co3flaBaa b cMecHTene paspeaceHne b 0,3-0,8 aTM. Ckopoctb nona-uh cnupTOBoro pacTBopa h ckopoctb yflaneHHH napos cnnpTa h boru perynHpyioTT3KHM o6pa3OM, HTo6bI COflep»aHHe JKHflKOft φβ3Μ B peaKHHOHHOň Macce BO BpeMHnonann pacTBopa cocTaBnnno 10-60% Mace,, npennoHTHTenbHO 30-40% Mace. Πρκco6niofleHHH yKa3aHHoro ycnoBHH He HaCntonaeTCH HanHnaHHH peaKUHOHHoň MaccwHa cTeHKH h nonacTH.CMecHTenH h oÓpaaoBaHUH komkob neneBoro nponyKTa. ΠοΟΚΟΗΗβΗΗΗ flOSHpOBaHHH cnupTOBoro paCTBOpa H3 peaKIÍHOHHOň Maccbl OTrOHHtÓT oc-T3TKH cnHPTa no coflepMaHHfl JieTynHx BemecTB no 0,5% h oxnawnaioT nonyneHHbiftnponyKT no KOMHaTHoň TeMnepaTypw. 260013 -3-
UeneBoň nponyxT nonyaaioT b BHne cyxoro TOHKonHcnepcHoro nopomxa, conepxa-mero 95γ99% οοηοβηογο BentecTBa. Bhxoa nponyxTa KOJiHuecTBeHHbiřr. BnnaHHe kojih-qecTBa menoaH Ha oocTaB nponyxTa πρκΒβηβΗο b TaOjnme 1. I a 6 ji h « a 1
ΙΐΒΜβΗβΗΗβ xanecTBa nponyxTa πρκ xpaHeHHH
MonbHoe cooTHome-ΗΗβ φτβ-JIHMHna H ΓΗηρΟΧΟΗ- na xanna ConepxaHHe neTynHxBeniecTB, % ConepxaHHe φτβηΗΜΗηβ Karmamorana b neneBOM nponyxTe, cpox xpaHeHHH, cyTKH Η φτ3— %, Hanano xoHen 0 30 60 * 120 1:0,95 0,23 . 0,42 91,8/7,7 91,4/7,8 91,0/8,3 90,3/8,2 1:1,00 0,26 0,44 93,3/5,5 92,6/4,4 - 88,1/5,5 1:1,02 0,33 0,34 96,8/0,4 94,6/0,9 - 82,5/1,3 1:1,03 0,33 0,39 97,2/1,0 97,4/1,3 97,0/1,5 97,1/1,5 1:1,05 0,51 0,50 96,5/0,8 96,1/1,1 96,9/0,9 96,6/0,7 1:1,10 0,36 0,38 96,4/otc. 97,5/otc. 96,6/0,4 97,0/0,3 1:1,03 0,27 0,27 98,5/0,3 98,9/0,2 98,6/0,3 98,5/0,2 (npHMep 1) 1:1,03 0,10 0,15 99,3/0,5 98,9/0,8 99,1/0,6 99,1/0,6 (npHMep 5)
Ha npHBeAeHHUx b TaCjiHue 1 flaHHbix bhzího, hto HajiHHHe b yeneBOM nponyxTecsočoňHoit qenotm He yBemraHBaeT γηγροοκοπηβηοοτβ nponyxTa h conepxaHnenetyranc coeflHHeHnň b npoyecce xpaHeHHH ocTaeTca HeHSMeHHUM. IIpoflyKT, no-nyneHHuň πρκ οτβχκοΜβτρΗΗβοκοΜ κοπΗΗβοτΒβ HHaCbiTxemenoHH MeHee 0,03 Moneft,HecTaCaneH πρκ xpaHeHHH. nponyxT, nonyneHHbiň πρκ Η36ωτκβ menoan 0,03 mojib ηBbmie, cTafouieH πρκ xpaHeHHH h no HCTeueHHH 120 cyToic conepxaHHe οοηοβηογοsenecTBa b ΗβΜ npaxŤHHecxH He Η3ΜβΗΗβτοΗ, Προηγκτ, nonyaeHHwií b ycnoBHaxnpHMepoB 1 h 5, no conepxaHioo οοηοβηογο BemecTBa, coflepxaHHra HenpopearapoBaB-pero φτβπκΜΗηη h CTaÓHjihHocTH πρκ xpaneHHH, ne ycTynaeT npoflyKTy, nonyaeHHd-My b ycjioBHHX npoTorana.
TaxHM oSpaaoM, H3 πρΗΒβηβΗΗΜΧ n&HHbix cnenyeT, mto He6onwnoft h36mtok cbo-CoffHoft menoHH (0,03 Mona mra 0,6% Mace.) ne tojimco He yxynmaeT xaaecTBo ne-neBoro nponyxTa, ho h cnocoCcTByeT ero Jiyqmeň coxpaHHOCTH πρκ ηπκτβηΒΗΟΜxpaHemra. H3o6peTeHHe Ηπηκ>οτρΗργβτθΗ cnenywmHMH npuMepaMH. IIpHMep 1. B cMecHTeni» raná Ββρκβρ-Πφπβϋηβρβρ βΜκοοτΜο 1,5 n, CHaCxeHHbiň py6amxoftnna oCorpeaa, repMeranHoft xpunucoft co urrynepaMH nna aarpyaxH peareHTOB h ot-’coca napoB, πρημμμ χοηοοηηβηηκομ η πρηθμηηκομ xoHneHcaTa, aarpyxaioT294,26 r (2 μοπη) φτβπΗΜΗήβ h npn nepeMemHBaHHH HarpeBawT no 75°C. TeMne-paTypy peaxnHOHHoft Maccbi HSMepatoT npn πομοπιη xpoMenb-Konenesofí TepMonapw,yxpenjieHHoň na xpunixe cMecHTena h norpyxeHHoii b peaxnHOHHyw Macey. K Harpe-ToMy ýTajiHMuny πρκ nepeMemHBaHHH’co cxopocTwo 15 γ/μηη nonawT pacTBop,cocToanraft H3 115,59 r (2,06 mojih) runpoKCHna xanna h 650 r CyTaHona. OnHo-speMeHHo b cMecHTene ycTaHaBJíHBBwT' paspexeHHe b 0,5-0,7 áTM. Ilapbi CyTaHonah sonbi, Bbip.ejiflionteftcH b nponecce BsaHMoneftcTBHa φτβπΗΜΗηβ c ΓκηΡοκοπηοΜ xa- 260013 -4- JIHH, KOHfleHCHpyiOT B XOJIOflHJIbHHKe H COSupaiOT B npHeMHHK. B npouecce flO3HpOB~kh cnnpTOBoro pacTBopa η οτγοηκη SyTaHona b peaKUHOHHOň Macce nonuepacHBaioTTeMnepaTypy b 70-75 C. Πρκ coSjnofleHHH ,yKa3aHHbix ycnoBHň peaKiiHOHHaa Maccab npouecce uoshpobkh pacTBopa npepiCTaBnaeT nnacTHHHyio nacTy u cojjepJKHT 35-40% SyTaHOJia. K KOHijy uo3hpobkh SyTaHonbHoro pacTBopa H3 peaxijHOHHoň MaccwOTroHHeTCH 400-450 r SyTaHona. ΠρΗ nepeMemHBaHHH h TeMnepaType 70-75°C bTeqeHHe 40-50 MHHyT οτγοηηιοτ ocTaBnmňcH SyTaHon, BbwepacHBaioT 10-20 MHHyT hoxjia»flaK)T peaKUHOHHyro Maccy flo 20-30°C. OTorHaHHbiň SyTaHon pereHepupytoT hHcnoJibayioT flna npoBefleHHH cnenywmeň onepaiiHH. IIonyaaioT 374,22 r MenKOKpHCTannHaecKoro nopomKa Seňoro UBeTa, conepacame-ro 98,5% οοηοβηογο Bem,ecTBa h 0,3% neTyaHX coeuHHeHHň. Bbixou nponyxTa 99,5%ot Teopnn, cnHTaa Ha 100% φτβηΗΜΜ,ιι κιπηη. flnHTejibHocTb npouecca cocTaBnaeT100-120 MHHyT, - ΠρΗΜβρ 2. B CMecHTenb 3arpyxaioT 294,26 r (2 mojih) Φτηκημη^β, repMeTH3HpyioT CMecH—Tejib, npH nepeMemHBaHHH HarpeBaioT φτβηΗΜΗΛ no TeMnepaTypbi 100-105°C, ycTa-HaBJíHBawT b CMecHTene pa3peweHHé b 0,3-0,5 aTM. h co ckopoctbio 17-18 γ/μηηnoflaioT pacTBop, cocToamraň H3 115,59 r rHUPOKciwa Kanna h 650 r SyTaHona. Bnpoijecce uo3HpoBaHHa pacTBopa η οτγοηκη SyTaHona b peaanHOHHoň Macce noflflep- -MHBaraT TeMneparypy 95-100°C, peaxiiHOHHaa Macca npeflcTaBnaeT cbmyayro nacTy,coflepMainyio 10—15% SyTaHona. K KOHiiy ηο3ηροβκη oTroHaeTca 580-610 r SyTaHo-na, B τβΗβΗΗβ 20-30 MHHyT πρκ nepeMemHBaHHH οτγοηηιοτ ocTaBmHíicH SyTaHon, na- 'k>t 10—MHHyTHyro BbiflepWKy h oxjiaxflaroT peaKUHOHHyio Maccy no 20-30°C. IIonyqaioT 378,26 r noponiKa Seňoro UBeTa, coflepxamero 95% ochobhoto BemecT-sa h 0,2% JieTýuHx coeuHHeHHň. Βωχοη nponyKTa cocTaBnaeT 97%, caHTaa Ha 100%φΤβΛΗΜΗβ KajIHH. ftnHTenbHocTb npouecca cocTasnaeT 75-85 MHHyT. ΠρΗΜβρ 3. B CMecHTenb 3arpy»awT 294,26 r (2 mojih) ,Φτηπημηαη, repMeTH3HpyioT cmcch—Tejib, npH nepeMemHBaHHH HarpeBaioT Φτηιιημηα no TeMnepaTypbi 55-60°C, ycTaHaB-jiHBaioT b CMecHTene pa3pexeHHe b 0,7-0,8 htm, h co ckopoctbio 12-13 γ/μηη no-uaioT pacTBop, cocToamHň hs 115,59 r rHflpoKCHua Kanna h 650 r SyTaHona. Bnpouecce uo3hpobkh pacTBopa η οτγοηκη 6yTaHona TeMnepaTypy peaKUHOHHOň Mac-cm noflflepJKHBaioT b npeuenax 50-55° C. K KOHuy uoshpobkh pacTBopa H3 peaKUHOH-hoíí. Macca οτγοηηθτοη 150-200 r SyTaHona h Macca npeflCTaBJíaeT nacTy, couep-Kamyio 55-60% SyTaHona, Πο οκοηηηηηη uoshpobkh b TeaeHHe 120-150 μηηυτ ot- 1roHHioT ocTaBmHňCH SyTaHon, uaioT 30-MHHyTHyio BbifíepacKy h oxnaatflaioT Maccy no20-30°C. . nojiynaioT 366,67 r nopomxa Seňoro UBeTa, coflepacamero 98% οοηοβηογο ee-mecTBa h 0,5% neTyaHx coepHHeHHň. Bbixofl cocTaBnaeT 97,5%, cnHTaa Ha 100%φτπηΗΜΗΑ Kanna, flnHŤenbHocTb npouecca cocTaBnaeT 210-220 MHHyT. npHMep 4. B ycnoBHHx npHwepa 1 H3 294,26 r (2 Moneň) φτβηπΜΗΉβ h 731,17 r.pacTBOrpa, coflepjKameró 231,17 r (2,06 μοπη) SyTHnaTa Kanna h 500 r SyTaHona h Har-peToro no 70°C, nonyaaioT 373,45 r nopomKa Seňoro UBeTa, coflepacamero 99,1%jocHOBHoro BemecTBa h 0,5% nerymix coeflHHeHHň. Bmxoh cocTaBnaeT 99,9%, chh-Tan Ha 1.00% Φτοπημηλ Kanna. npHMep 5. B ycnoBHax npHMepa 1 H3 294,26 r φτβπΗΜΗββ h 771,37 r pacTBopa, coctoh- mero Η3 100,81 r rnupoRCHua Kanna, 11,56 r Syranara xanna h 650 r SyTaHona, nonyaaioT 372,7 r nopomKa Seňoro UBeTa, coflepscamero 99,3% οοηοβηογο BemecT-
Ba h 0,1% neTyanx coeflHHeHHň. 260013 -5-
BbocoK cocTaBJíHeT 99,9%,CHHTaa Ha 100% φτβηκΜΗΑ xajiHH. ΠρΗΜβρ 6, B ycnoBHnx npHMepa 1 hs 294,26 r (2 Moneft) Φτ3πημηα& h pacTBopa 82 rrHflpoKCHfla HaTpuH b 600 r OyTaHona nonynaioT 346,95 r nopomxa 6enoro ΑΒβτβ,coflepxamero 97% Φτοπημηα& ηβτρηη η 0,3% neTy^mc coe^HHeHHň.
Bbixofl cocTaBJíHeT 99,5%, cwaH na 100% φτβηΗΜΗΑ HaTphn. ΠρΗΜβρ 7 B ycnoBHflx npHMepa 1 «3 294,26 γ φτβπκΜΗΑβ h 115,59 r nwpoKCHjoia xanHH,pacTBopeHFtoro b 650 r βτηποβογο cnupTa, ηοηγνβιοτ 374,27 r nopomxa BejioroιΧΒβτβ, conepxamero 97% ochobhoio semecTBa h 0,3% neTynHX.
Buxon cocTaBJíaeT 98%, οηητηη Ha 100% Φτηπημηα xanHH. ΠρΗΜβρ 8 B ycnoBHHx npHMepa 1 hs 294,26 r Φτθπημηαβ h 115,59 r rHAPOKCHMaxanHH,pacTBopeHHoro b 650 r κβοπροπηποβογο cnnpTa, nonynaioT 372,35 r nopomxa 6e-noro useta, conepxamero 98% οοηοβηογο BemecTBa h 0,1% neTyqHx.
Buxoa βοβτβΒΗΗβτ 98,5%, CHHTaa Ha 100% Φτηπημηα xanHH.
TaKHM oCpaaoM, npennaraeMMtt cnocofi nonyqeHHH φτβπΗΜΗΑΟΒ menoHHbix MeTan-noe nosBonneT cymecTBeHHo ynpocTHTb η ηητθηοηΦηαηροβητβ npouecc, ηοκηιοηητβCTaflHH φκηι>τροΒ8ΗΗΗ cycneHSHH h cymKH nacTbi, πηκβηαηροββτβ MexonepauHoHHyioTpaHcnopTHpoBxy πηπκοΗ Maxynteftcn nacTbi, sHauHTenbHo ynpocTHTb annapaTypHoeοφορΜπβΗΗβ npouecca, MexaHHSHpoBaTb h aBTOMaTHSHpoBaTb npopecc. Πρπ stomAJiHTejibHocTb npouecca nonyneHHH coxpaqaeTcn c 6-8 qacoe A° 1,5-3,5 qacoB. ΦΟΡΜΥΠΑ Η30ΒΡΕΤΕΗΗ»
Cnoco6 nonyneHHH Φτβπημηαοβ menomibix MeTannoB nyTeM B3anMoneftcTBHH φτβ-nHMHAa co cnuptoBUM pacTBopoM rHAPOKcHAa h/hjih ajiKorojiHTOM menoHHoro MeTannanpH TeMnepaType 50-l40eC,o TnHHawmHftCH τβΜ, hto, c uenbio ynpo-qeHHH η ΗΗΤβΗΟΗφΗκβιχΗΗ npouecca, BBaHMopeňcTBHe eeAyT πόα BaxyyMOM η βμαθπη-nqHecH napu cnHpTa h boom ynanmoT co cxopocŤb», oGecnenHBaiomeň b peaxuHOHHoťíMacce b npouecce ποαβηη οπηρτοβογο pacTBopa xoHueHTpauHio cnnpTa 10-60% Mace. HCTOMHHRH ΗΗφορΜβΑΗΗ, npHHHTbie BO BHHMaHHe npH 3KCnepTH3e: 1. MeTOAta sxcnepHMeHTa b opraHHnecxott xhmhh, M,, Xhmhh, 1969, c. 415. 2. ΠβτβΗΤ ΒβηΗκοβρκτβΗΗΗ > 1420523, xn. C 2 C, ony6n. 1976, 3. AsTopcKoe CBHAeTeJibCTBo CCCP ÍP 875794, M.xn.3 C 07 D 209/48, óny6n.(προτοτΗπ).
P E Φ E P A T
CnOCOB ,ΠΟΠΪΗΕΗΗΗ ΦΤΑΠΗΜΗΠΟΒ ΠΙΕΠΟΗΗΝΧ METAJUIOB
Cnoco6 noJiyneHHH φτβηκΜΗΑΟΒ mejioUHbix MeTannoB saxmonaeTCH bo ββηημο—AeňCTBHH ΦΤ8ΠΗΜΗΑ& CO CAHPTOBblM paCTBOpOM rHAPOKCHMa h/hUH ΒΠΚΟΓΟΠΗΤΟΜmejioHHoro MeTanna ποα BaxyyMOM npH TeMnepaType 50-l40flC. BunennioinHecH npHpeaKipm napu cnupra h boau ynannioT co cxopoCTbto, oOecneHHBawmeň b peaxuHOH-Hoň Macce b npouecce nouauH cnnpTOBoro pacTBopa KOHueHTpaumo οπκρτβ 10-60 % Mace. npHSHaHo ΗΒοΟρβτβΗΗβΜ no peaynbTaTaM^SKcnepTHShi, ocymecTBněHHoft TocynapcT-ΒβΗΗΜΜ ΚοΜΗΤΘΤΟΜ CCCP ΠΟ ΑβΠβΜ Η3θ6ρβΤβΗΗή H OTKpMTHň. 260013
Claims (1)
- -6- PŘEDMŽT VYNALEZU Způsob výroby ftalimidů alkalických kovů vzájemnýmpůsobením ftalimidů s alkoholickým roztokem hydroxidua/nebo alkoholátem alkalického kovu při teplotě 50 až140 °C, vyznačující se tím, že se reakce provádí ve vakuua vznikající páry alkoholu a vody se odstraňují rychlostizajištující v reakční hmotě pro přívod alkoholického rozto-ku koncentraci alkoholu 10 až 60 % hmot. 260013
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS843729A CS260013B1 (cs) | 1984-05-18 | 1984-05-18 | Způsob výroby ftalimidů alkalických kovů |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS843729A CS260013B1 (cs) | 1984-05-18 | 1984-05-18 | Způsob výroby ftalimidů alkalických kovů |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS372984A1 CS372984A1 (en) | 1987-06-11 |
| CS260013B1 true CS260013B1 (cs) | 1988-11-15 |
Family
ID=5378197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS843729A CS260013B1 (cs) | 1984-05-18 | 1984-05-18 | Způsob výroby ftalimidů alkalických kovů |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS260013B1 (cs) |
-
1984
- 1984-05-18 CS CS843729A patent/CS260013B1/cs unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CS372984A1 (en) | 1987-06-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA1085619A (en) | Method of selectively recovering molybdenum from aqueous solutions thereof | |
| CS227668B2 (en) | Preparation of cycloalcanols and cycloalcanons | |
| KR970706404A (ko) | 유기상내로의 추출에 의한 소수성 증폭 생성물의 검출 방법(detection of hydrophobic amplification products by extraction into an organic phase) | |
| CS260013B1 (cs) | Způsob výroby ftalimidů alkalických kovů | |
| McClelland | Benzamide oxygen exchange concurrent with acid hydrolysis | |
| KR940005551A (ko) | 2,5-디-페닐아미노-테레프탈산 및 그의 디알킬 에스테르의 제조방법 | |
| Balsamo et al. | Anomalous steric course of ring opening reactions of indene oxide. Reexamination | |
| CN100408585C (zh) | 制造硅烷醇封端的低聚材料的方法 | |
| CA1249846A (en) | Method for the rearrangement of dialkylbenzene dihydroperoxides to dihydric phenols | |
| Blank et al. | Deoxygenation of 1, 4-epoxides by Grignard reagents | |
| IE35378B1 (en) | Erythromycylamine compounds | |
| IE38743B1 (en) | Improved incandescent lamp | |
| Brooks et al. | The Preparation of Benzoyl Hydrogen Peroxide | |
| JPS5513702A (en) | Preparation of polyoxysulfone | |
| Schäfer et al. | Cyclic response of energy linked functions of liver Mitochondria to uncoupling thiophene derivatives | |
| GB1494161A (en) | Stabilised halogenotriazine dyestuff preparations | |
| Perez et al. | Kinetics of gas‐phase thermal elimination of (α‐phenylethyl) and (β‐phenylethyl)‐pyrazole | |
| JPS6056163B2 (ja) | ポリブタジエンのエポキシ化方法 | |
| JP2003511433A5 (cs) | ||
| US3171854A (en) | Preparation of phenyl o-halobenzoates and conversion thereof to phenol | |
| US698761A (en) | Process of producing camphor. | |
| Shackelford et al. | A Novel reaction of xenon trioxide. Organic. pi. bond epoxidation. II. Concerning the Mechanism | |
| US629433A (en) | Process of making alkyl ethers of morphin. | |
| KR960022540A (ko) | 인산에스테르 화합물의 제조방법 | |
| Browne | The Influence of Hydroxy Acids and Lactones upon Determinations of the Chemical Constants of Fatty Acids. |