PL90027B1 - - Google Patents

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PL90027B1
PL90027B1 PL1970173770A PL17377070A PL90027B1 PL 90027 B1 PL90027 B1 PL 90027B1 PL 1970173770 A PL1970173770 A PL 1970173770A PL 17377070 A PL17377070 A PL 17377070A PL 90027 B1 PL90027 B1 PL 90027B1
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/13Amines
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/13Amines
    • A61K31/135Amines having aromatic rings, e.g. ketamine, nortriptyline
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/275Nitriles; Isonitriles
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P25/00Drugs for disorders of the nervous system
    • A61P25/02Drugs for disorders of the nervous system for peripheral neuropathies
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • A61P9/06Antiarrhythmics
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • A61P9/08Vasodilators for multiple indications
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • A61P9/10Drugs for disorders of the cardiovascular system for treating ischaemic or atherosclerotic diseases, e.g. antianginal drugs, coronary vasodilators, drugs for myocardial infarction, retinopathy, cerebrovascula insufficiency, renal arteriosclerosis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • A61P9/12Antihypertensives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C233/00Carboxylic acid amides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C255/00Carboxylic acid nitriles
    • C07C255/49Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
    • C07C255/53Carboxylic acid nitriles having cyano groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing cyano groups and hydroxy groups bound to the carbon skeleton
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04HBUILDINGS OR LIKE STRUCTURES FOR PARTICULAR PURPOSES; SWIMMING OR SPLASH BATHS OR POOLS; MASTS; FENCING; TENTS OR CANOPIES, IN GENERAL
    • E04H13/00Monuments; Tombs; Burial vaults; Columbaria
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/55Design of synthesis routes, e.g. reducing the use of auxiliary or protecting groups

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  • Bioinformatics & Cheminformatics (AREA)
  • General Chemical & Material Sciences (AREA)
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  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Heart & Thoracic Surgery (AREA)
  • Cardiology (AREA)
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  • Urology & Nephrology (AREA)
  • Biomedical Technology (AREA)
  • Neurology (AREA)
  • Neurosurgery (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Hydrogenated Pyridines (AREA)

Description

Przedmiotem wynalazku jest sposób wytwarzania nowych racemicznych lub optycznie czynnych 1-feno- ksy-2-hydroksy-3-cykloalkiloaminopropanów i ich soli addycyjnych z kwasami.Nowym zwiazkom odpowiada wzór 1, w którym R oznacza grupe alkilowa, zawierajaca do 5 atomów wegla, Ri oznacza grupe nitrylowa (-C^N), lub chlorowiec, R2 oznacza wodór, chlorowiec, grupe nitrylowa lub grupe alkilowa, alkoksylowa lub alkenylowa, zawierajaca do 5 atomów wegla, R3 oznacza wodór, chlorowiec, grupe alkilowa lub alkoksylowa, zawierajaca do 5 atomów wegla i n oznacza liczbe calkowita 2-7.Nowe zwiazki wytwarza sie wedlug wynalazku, przez dwuazowanie zwiazku o wzorze 2, w którym R, R2 i R3 i n maja wyzej podane znaczenie i ogrzewanie z cyjankiem miedziawym wzglednie z halogenkiem miedzia- wym.Zwiazki o wzorze 2 zawieraja juz gotowy szkielet 1-fenoksy-2-hydroksy-3-cykloalkiloaminopropanu i'mozna je wytwarzac wychodzac z odpowiedniego fenolu, który poddaje sie reakcji z epichlorohydryna i utworzony 1-fenoksy-2,3-epoksypropan wprowadza w reakcje z cykloalkiloamina.Zwiazki otrzymywane sposobem wedlug wynalazku posiadaja asymetryczny atom wegla w grupie CHOH i wskutek tego wystepuja jako racematy i w postaci optycznych antypodów. Te ostatnie mozna otrzymac przez rozdzielenie racematu za pomoca zwykle uzywanych kwasów pomocniczych, takich jak kwas dwubenzoilo-D^ • winowy lub kwas D-3-bromokamforo-8-sulfonowy, jak równiez przez stosowanie optycznie czynnych zwiazków wyjsciowych.Otrzymywane sposobem wedlug wynalazku 1-fenoksy-3-cykloaminopropanole o wzorze 1 mozna w znany sposób przeprowadzic w fizjologicznie dopuszczalne sole addycyjne z kwasami. Odpowiednimi kwasami sa: kwas solny, kwas bromowodorowy, kwas siarkowy, kwas metanosulfonowy, kwas maleinowy, kwas octowy, kwas szczawiowy, kwas mlekowy, kwas winowy lub 8-chloroteofilina.Zwiazki o wzorze 1 wzglednie ich fizjologicznie dopuszczalne sole addycyjne z kwasami wykazuja w badaniach na swinkach morskich, jako zwierzetach doswiadczalnych, wartosciowe wlasciwosci terapeutyczne, w szczególnosci dzialanie 0-adrenolityczne i mozna je wskutek tego stosowac do leczenia i profilaktyki schorzen naczyn wiencowych serca i arytmii serca, zwlaszcza tachycardii, w medycynie. Równiez dzialanie obnizajace2 90027 cisnienie krwi jest pod wzgledem terapeutycznym interesujace.Szczególnie wartosciowymi sa przy tym takie zwiazki o wzorze 1, w którym R oznacza grupe metylowa, R3 i R3 oznaczaja zwlaszcza wodór, a równiez grupe alkilowa i Rt oznacza przede wszystkim grupe nitrylowa (w szczególnosci w polozeniu 2 lancucha propanolowego) i n ¦ 4, 5 lub 6. Równiez, gdy R oznacza grupe metylowa, Ri oznacza chlorowiec, a R2 oznacza wodór, lub grupe metylowa, a R3 oznacza wodór, a n ¦ 4,5 lub 6 zwiazki wykazuja silne dzialanie 0-adrenoJityczne. Szczególnie wartosciowymi pod wzgledem terapeutycznym sa: 1-(2-nitrylofenoksy)-2-hydroksy-3-(1-metylocyklopentylo)-aminopropan oraz 1-(2-nitrylofenoksy)-2-hydro- ksy-3-(1-metylocykloheksylo)-aminopropan, 1-(2-chloro-5-metylofenoksy)-2-hydroksy-3-(1-metylocyklopenty*- lo)-aminopropan i 1-(2-bromofenoksy)-2-hydroksy-3-(1-metylocykloheptylo)-aminopropan wzglednie Ich fizjolo¬ gicznie dopuszczalne lole addycyjna z kwitami, 1-(2-nltrylofanokiy)-2-hydrokiy-3-(1-metylocykloptntylo)-imlno- \-propan Jest izczagólnle Interesujacym wskutek twego znacznego dzialania mtagonlttyczntgo wobec Izoprotere- nolu, przy prawie calkowitym brak wlasnego dzialania powodujacego rzadkoskurcz. Szczególnie aktywnymi sa zwiazki, które w grupie fenylowej sa podstawione grupa nitrylowa w polozeniu 2 i równoczesnie nizsza grupa alkilowa, zwlaszcza metylowa w polozeniu 5, np. 1-(2-nitrylo-5-metylofenoksyy-2-hydroksy-3-(1-metylocyklop- entyloamino)-propan, 1-(2-nitrvlo-5-metvlofenoksy)2-hydroksy-3-(1-metylocykloheksyloamino)-propan i 1-(2-nt* trylo-5-metylofenoksy)-2-hydroksy-3-(1-metylocykloheptyloamino)-propan, wzglednie fizjologicznie dopuszcza¬ lne sole addycyjne tych zwiazków z kwasami.Dawka jednostkowa zwiazków otrzymywanych sposobem wedlug wynalazku wynosi 1—300 mg, zwlaszcza —100 mg (doustnie) lub 1—20 mg (pozajelitowo).Galenowa obróbke zwiazków otrzymywanych sposobem wedlug wynalazku do zwykle uzywanych form uzytkowych, takich jak roztwory, emulsje, tabletki, drazetki lub preparaty o przedluzonym dzialaniu, przepro¬ wadza sie w znany sposób, stosujac zwykle galenowe srodki pomocnicze, nosniki, srodki rozkruszajace, wiazace' lub poslizgowe, substancje smakowe, slodzace, srodki do powodowania przedluznego dzialania i ulatwiajace- rozpuszczanie.Otrzymywane sposobem wedlug wynalazku zwiazki mozna laczyc z innymi substancjami o dzialaniu farmakodynamicznym, takimi, jak np. srodki rozszerzajace naczynia wiencowe, sympatikomimetyczne, glikozydy nasercowe lub srodki uspokajajace.Przyklad I. Chlorowodorek 1-(2-cyjanofenoksy)-2-hydroksy-3-(1-metylocykloheksyloamino)-prcpanu.Do goracego roztworu z 5 g siarczanu miedzi, 5,8 g cyjanku miedzi i 30 ml wody powoli wkrapla sie roztwór soli dwuazoniowej, wytworzonej z 3,52 g (0,01 mola) chlorowodorku 1-(2-aminofenoksy)-2-hydroksy-3- (l-metylocykloheksyloamino)-propanu, 4 ml stezonego HCI, 20 ml wody i wodnego roztworu 1,4 g (0,01 mola) NaN02. Po 30 minutach mieszania w temperaturze 90°C oziebia sie ialkalizuje za pomoca NaOH. Po dodaniu chloroformu oddziela sie nierozpuszczalne czesci. Faze organiczna wyodrebnia sie, przemywa woda i suszy nad MgS04. Po oddestylowaniu CHCI3 pozostalosc rozpuszcza sie w etanolu i dodaje eterowy roztwór HCI.Wytracajace sie krysztaly przekrystalizowuje sie jeszcze raz w etanolu dodajac eter. Wydajnosc: 950 mg.Temperaturatopnienia: 161—164°C.Przyklad II. Chlorowodorek 1-(2-nJtrylofenoksy)-2-hydroksy-3-(1-metylocykloheksyloamino)-proparW, * 3,52 g (0,01 mola) chlorowodorku 1-(2-aminofenoksy)-2-hydroksy-3-(1-metylocykloheksyloamino)-pro- cpanu rozpuszcza sie w 20 ml H20 i 4 ml stezonego HCI. 1,4 g (0,02 mola) NaN02 rozpuszcza sie w 5 ml wody i powoli wkrapla sie do roztworu aminy. Przez chlodzenie lodem utrzymuje sie temperature 0° do +5°C. Po zakonczeniu dodawania utrzymuje sie roztwór jeszcze przez 15 minut w temperaturze okolo 0°C. 5g CuS04 x 5H20 (0,02 mola), 5,8 g KCN (0,04 mola) i 30 ml H2 O laczy sie i mieszajac ogrzewa do 90°C.Roztwór dwuazoniowy miesza sie z goracym roztworem Cu/I/CN i calosc utrzymuje sie przez 30 minut w temperaturze 90°C. Po oziebieniu i zadaniu 10% roztworem NaOH ekstrahuje sie chloroformem. Roztwór CHCI3 przemywa sie woda, suszy nad MgS04 i zateza. Pozostalosc rozpuszcza sie w etanolu i zakwasza alkoholowym roztworem HCI. Po dodaniu eteru produkt wykrystalizowuje. Po jeszcze jednym przekrystalizo- waniu z ukladu alkohol/eter otrzymuje sie 950 mg produktu, o temperaturze topnienia: 161—163°C.Przyklad III. Chlorowodorek 1-(2-nitrylo-5-metylofenoksy)-2-hydroksy-3-(1-metylocykloheksyloam- ino)- propanu. 2,92 g (0,01 mola) 1-(2-amino-5-metylofenoksy)-2-hydroksy-3-(1-metylocykloheksyloamino)-propanu roz¬ puszcza sie w 20 ml wody i 6 ml stezonego HCI. 1,4 g (0,02 mola) NaN02 rozpuszcza sie w 5 ml wody i powoli wkrapla podczas mieszania do roztworu aminy. Przez oziebianie lodem utrzymuje sie temperature 0° do +5°C.Po zakonczeniu dodawania roztwór utrzymuje sie przez 15 minut w temperaturze okolo 0°C. g CuS04 X 5H20 (0,02 mola), 5,8 g KCN (0,09 mola) i 30 ml H2 O laczy sie i podczas mieszania ogrzewa90027 3 do temperatury 90°C. Roztwór dwuazoniowy wkrapla sie podczas mieszania do goracego roztworu Cu/I/CN i pozostawia przez 30 minut w temperaturze 90°C do przereagowania. Po oziebieniu i zadaniu 10% NaOH ekstrahuje sie chloroformem. Ekstrakt chloroformowy przemywa sie woda, suszy nad MgS04 izateza.Pozostalosc rozpuszcza sie wacetonitrylu i zakwasza alkoholowym roztworem HCI. Wykrystalizowany chloro¬ wodorek przekrystalizowuje sie jeszcze raz z acetonitrylu. Temperatura topnienia: 170-173°C, wydajnosc: 500 mg.Analogicznie, jak w wyzej podanych przykladach, wytwarza sie nastepujace zwiazki o wzorze 1: Temperaturatopnienia Temperaturatopnienia Rt R, Rf R n °C (chlorowodorek) 2-Br 2-a 2-Br 2-Br 2-a 2-a 2<:n ^CN 2-a 2-CN 2-CN 2-CN 2-CN 2-CN H "CsH, H II -CHj -CH, H H -CH, H 4-a -CH, -ch, H H H H H H H H H H H H H H H CH, CH, CH, CH, CH, C2H5 C,H5 i-C,H7 CH, CH, CH, CH, CH, CH, 4 4 6 6 6 6 4 4 156-157 170-172 157-158 167-168 174-177 179-180 157-158 200-201 191-194 160-161 194-196 192-194 143-146 132-134 ^ 2 II R WZ0R 1 ^73^0CH2-CH0H-CH2-NH-CjCH2)n WZ0R2 Prac. Poligraf. UP PRL naklad 120+18 Cena 10 zl PL PL PL PL PL PLThe subject of the invention is a process for the preparation of new racemic or optically active 1-phenoxy-2-hydroxy-3-cycloalkylaminopropanes and their acid addition salts. The new compounds correspond to formula 1, in which R is an alkyl group containing up to 5 carbon atoms, Ri is nitrile (-C1N), or halogen, R2 is hydrogen, halogen, nitrile or an alkyl, alkoxy or alkenyl group of up to 5 carbon atoms, R3 is hydrogen, halogen, alkyl or alkoxy of up to 5 atoms carbon and n is an integer of 2-7. The new compounds are prepared according to the invention by diazotizing a compound of formula 2, wherein R, R2 and R3 and n are as defined above, and heating with cuprous cyanide or with a cuprous halide. 2 already contain the ready skeleton of 1-phenoxy-2-hydroxy-3-cycloalkylaminopropane and can be prepared starting from the corresponding phenol, which is reacted with epichlorohydrin and formed 1-phenoxy-2,3 -epoxypropane is reacted with cycloalkylamine. The compounds according to the invention have an asymmetric carbon atom in the CHOH group and therefore occur as racemates and in the form of optical antipodes. The latter can be obtained by resolving the racemate with the usual auxiliary acids, such as dibenzoyl-D 4 -tartaric acid or D-3-bromocamphor-8-sulfonic acid, as well as by using optically active starting compounds. The phenoxy-3-cycloaminopropanols of the formula I can be converted into physiologically acceptable acid addition salts in a known manner. Suitable acids are: hydrochloric acid, hydrobromic acid, sulfuric acid, methanesulfonic acid, maleic acid, acetic acid, oxalic acid, lactic acid, tartaric acid or 8-chlorothophyllin. Compounds of formula I or their physiologically acceptable acid addition salts show in tests in guinea pigs, as experimental animals, valuable therapeutic properties, in particular o-blocking activity, and can therefore be used for the treatment and prevention of coronary artery diseases and cardiac arrhythmias, especially tachycardia, in medicine. The blood pressure lowering effect2 90027 is also therapeutically interesting, especially the compounds of formula I in which R is methyl, R3 and R3 are especially hydrogen, and the alkyl group and Rt are primarily the nitrile group (in especially in the 2-position of the propanol chain) and n 4, 5 or 6. Also, when R is methyl, Ri is halogen and R2 is hydrogen or methyl and R3 is hydrogen, and n ¦ 4,5 or 6 the compounds show strong 0-adrenaline action. Therapeutically valuable are: 1- (2-nitrilophenoxy) -2-hydroxy-3- (1-methylcyclopentyl) -aminopropane and 1- (2-nitrilephenoxy) -2-hydroxy-3- (1-methylcyclohexyl) -aminopropane, 1- (2-chloro-5-methylphenoxy) -2-hydroxy-3- (1-methylcyclopenty * yl) -aminopropane and 1- (2-bromophenoxy) -2-hydroxy-3- (1-methylcycloheptyl) ) -aminopropane or their physiologically acceptable flower additive, 1- (2-nltrilophanokiy) -2-hydroxyy-3- (1-methylcyclopentyl) -imyl-1-propane is especially interesting due to its considerable mtagglottic action against isoprotective compounds. nole, with almost complete absence of its own bradycardia effect. Particularly active are compounds which in the phenyl group are substituted with a nitrile group in position 2 and, at the same time, with a lower alkyl group, especially methyl in position 5, e.g. 1- (2-nitrile-5-methylphenoxy-2-hydroxy-3- (1- methylcyclopentylamino) propane, 1- (2-nitril-5-methylphenoxy) 2-hydroxy-3- (1-methylcyclohexylamino) propane and 1- (2-nt * tryl-5-methylphenoxy) -2-hydroxy- 3- (1-methylcycloheptylamino) -propane, relatively physiologically acceptable acid addition salts of these compounds with acids. The unit dose of the compounds according to the invention is 1-300 mg, especially 100 mg (orally) or 1-20 mg (parenterally). The galenic treatment of the compounds according to the invention into the usual use forms, such as solutions, emulsions, tablets, dragees or long-acting preparations, is carried out in a known manner, usually using galenic auxiliaries, carriers, disintegrants, binders. or lubricants, flavors, sweeteners, sro Prolonging and dissolving agents. The compounds obtained according to the invention can be combined with other substances having a pharmacodynamic effect, such as e.g. coronary vasodilators, sympathomimetic agents, cardiac glycosides or sedatives. Example 1- 2. -cyanophenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) -prcpan. To a hot solution of 5 g of copper sulphate, 5.8 g of copper cyanide and 30 ml of water is slowly added dropwise the solution of the diazonium salt prepared from 3.52 g (0.01 mol) 1- (2-aminophenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) propane hydrochloride, 4 ml concentrated HCl, 20 ml water and an aqueous solution of 1.4 g (0.01 mol) NaN02. After 30 minutes of stirring at 90 ° C, it is cooled and made alkaline with NaOH. When chloroform is added, the insoluble matter is separated. The organic phase is separated, washed with water and dried over MgSO 4. After CHCl 3 has been distilled off, the residue is dissolved in ethanol and ethereal HCl is added. The crystallizing crystals are recrystallized once more in ethanol while adding ether. Yield: 950 mg. Melting point: 161-164 ° C. Example II. 1- (2-N-ethylphenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) -proparW hydrochloride, * 3.52 g (0.01 mol) 1- (2-aminophenoxy) -2-hydroxy-3- ( 1-methylcyclohexylamino) propane is dissolved in 20 ml of H 2 O and 4 ml of concentrated HCl. 1.4 g (0.02 mol) of NaNO 2 are dissolved in 5 ml of water and slowly added dropwise to the amine solution. The temperature is kept at 0 ° to + 5 ° C by cooling with ice. After the addition is complete, the solution is kept for an additional 15 minutes at a temperature of approximately 0 ° C. 5 g of CuSO 4 x 5H 2 O (0.02 mol), 5.8 g of KCN (0.04 mol) and 30 ml of H 2 O are combined and heated to 90 ° C with stirring. The diazonium solution is mixed with the hot Cu / I / CN solution and The whole thing is kept for 30 minutes at a temperature of 90 ° C. After cooling and treating with 10% NaOH solution, extraction was carried out with chloroform. The CHCl3 solution is washed with water, dried over MgSO4 and concentrated. The residue is dissolved in ethanol and acidified with an alcoholic HCl solution. Upon addition of ether, the product crystallizes out. After a further recrystallization from the alcohol / ether system, 950 mg of product are obtained, mp: 161-163 ° C. Example III. 1- (2-Nitrile-5-methylphenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) propane hydrochloride. 2.92 g (0.01 mol) of 1- (2-amino-5-methylphenoxy) -2-hydroxy-3- (1-methylcyclohexylamino) propane were dissolved in 20 ml of water and 6 ml of concentrated HCl. 1.4 g (0.02 mol) of NaNO 2 are dissolved in 5 ml of water and slowly added dropwise with stirring to the amine solution. The temperature is kept at 0 ° to + 5 ° C by cooling with ice. After the addition is complete, the solution is kept at a temperature of about 0 ° C for 15 minutes. g of CuSO 4 X 5 H 2 O (0.02 mol), 5.8 g of KCN (0.09 mol) and 30 ml of H 2 O are combined and, with stirring, heated to 90 ° C. The diazonium solution is added dropwise to the hot Cu / I / CN solution with stirring and left to react for 30 minutes at 90 ° C. After cooling and quenching with 10% NaOH, extraction was carried out with chloroform. The chloroform extract is washed with water, dried over MgSO 4 and dried. The remainder is dissolved in acetonitrile and acidified with an alcoholic HCl solution. The hydrochloride that crystallizes out is recrystallized once more from acetonitrile. Melting point: 170-173 ° C, yield: 500 mg By analogy to the examples above, the following compounds of formula 1 are prepared: Melting point Melting point Rt R, Rf R n ° C (hydrochloride) 2-Br 2-a 2 -Br 2-Br 2-a 2-a 2?: N ^ CN 2-a 2-CN 2-CN 2-CN 2-CN 2-CN H "CsH, H II -CHj -CH, HH -CH, H 4-a -CH, -ch, HHHHHHHHHHHHHHH CH, CH, CH, CH, CH, C2H5 C, H5 iC, H7 CH, CH, CH, CH, CH, CH, 4 4 6 6 6 6 4 4 156- 157 170-172 157-158 167-168 174-177 179-180 157-158 200-201 191-194 160-161 194-196 192-194 143-146 132-134 ^ 2 II R WZ0R 1 ^ 73 ^ 0CH2 -CH0H-CH2-NH-CjCH2) n WZ0R2 Printing UP PRL Edition 120 + 18 Price PLN 10 PL PL PL PL PL PL

Claims (2)

1. Zastrzezenie patentowe 1. Sposób wytwarzania nowych 1-fenoksy-2-hydroksy-3-cykloalkiloaminopropanów o wzorze 1, w którym R oznacza grupe alkilowa, zawierajaca do 5 atomów wegla, R, oznacza grupe nitrylowa lub chlorowiec, R2 oznacza wodór, chlorowiec, grupe nitrylowa lub grupe alkilowa, alkoksylowa lub alkenyIowa, zawierajaca do ,5 atomów wegla, R3 oznacza wodór, chlorowiec, grupe alkilowa lub alkoksylowa, zawierajaca do 5 atomów wegla i n oznacza liczbe calkowita1. Claim 1. A method for the preparation of the new 1-phenoxy-2-hydroxy-3-cycloalkylaminopropanes of formula 1, in which R is an alkyl group of up to 5 carbon atoms, R is a nitrile or halogen group, R2 is hydrogen, halogen , nitrile or alkyl, alkoxy or alkenyl group of up to 5 carbon atoms, R3 is hydrogen, halogen, alkyl or alkoxy of up to 5 carbon atoms and n is an integer 2. -7, w postaci racematu lub izomerów optycznie czynnych oraz ich fizjologicznie dopuszczalnych soli addycyjnych z kwasami, znamienny tym, ze zwiazek o wzorze 2, w którym R, R2 i R3 i n maja wyzej podane znaczenie, dwuazuje sie i poddaje reakcji z cyjankiem miedziawym lub halogenkiem miedziawym i otrzymany zwiazek o wzorze 1, o ile wystepuje w postaci racematu, ewentualnie przeprowadza w diastereomeryczne sole za pomoca odpowiednich kwasów pomocniczych, i te ostatnie rozdziela sie na drodze frakcjonowanej krystalizacji i zwiazki o wzorze 1 ewentualnie przeprowadza w ich fizjologicznie dopuszczalne sole addycyjne z kwasami.90 027 OCK-CHOH-CH-NH-n&H,),, i 2 Nw* PL PL PL PL PL PL2.-7, in the form of the racemate or optically active isomers and their physiologically acceptable acid addition salts, characterized in that the compound of formula II, wherein R, R2 and R3 and n are as defined above, are diazotized and reacted with cyanide cuprous or cuprous halide and the resulting compound of formula I, if present in the form of a racemate, is optionally converted into diastereomeric salts with suitable auxiliary acids, and the latter are separated by fractional crystallization and the compounds of formula I are optionally converted into their physiologically acceptable salts acid addition. 90 027 OCK-CHOH-CH-NH-n & H,) ,, and 2 Nw * PL PL PL PL PL PL
PL1970173770A 1969-07-23 1970-07-21 PL90027B1 (en)

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DE1937477A DE1937477C3 (en) 1969-07-23 1969-07-23 I-phenoxy-2-hydroxy-3- (l -methylcycloalkylamino) propane, process for their preparation and medicaments containing them

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US4021576A (en) * 1969-07-23 1977-05-03 Boehringer Ingelheim Gmbh Pharmaceutical compositions containing a 1-(2'-ethynyl-phenoxy)-2-hydroxy-3-(cycloalkyl-amino)-propane and method of use
US3937706A (en) * 1969-07-23 1976-02-10 Boehringer Ingelheim Gmbh 1-(2'ethynyl-phenoxy)-2-hydroxy-3-(cycloalkyl-amino)-propanes and salts thereof
US4120978A (en) * 1970-01-08 1978-10-17 Ciba-Geigy Corporation Pharmaceutical composition for inhibiting and blocking cardioselective beta-receptors
US4038313A (en) * 1970-01-08 1977-07-26 Ciba-Geigy Corporation Cycloalkylureido phenoxy propanolamines
SE354851B (en) * 1970-02-18 1973-03-26 Haessle Ab
US4145442A (en) * 1972-04-04 1979-03-20 Aktiebolaget Hassle Phenoxy-hydroxypropylamines, their preparation, and method and pharmaceutical preparations for treating cardiovascular diseases
US4038414A (en) * 1972-06-08 1977-07-26 Ciba-Geigy Corporation Amines and processes for their manufacture
US4035420A (en) * 1972-07-06 1977-07-12 Aktiebolaget Hassle Substituted ureido alkylene phenoxy propanolamines
DE2309887C2 (en) * 1973-02-28 1983-11-10 C.H. Boehringer Sohn, 6507 Ingelheim 1-aryloxy-2-hydroxy-3-alkynylaminopropane derivatives and their physiologically acceptable acid addition salts, pharmaceutical preparations and manufacturing processes for the compounds
US4220659A (en) * 1974-02-22 1980-09-02 Boehringer Ingelheim Gmbh 1-Phenoxy-2-hydroxy-3-alkynylamino-propanes and salts thereof
DE2540552A1 (en) * 1974-09-12 1976-03-25 American Cyanamid Co CYCLOALKYL DERIVATIVES OF 1-ARYLOXY-3-AMINO-2-PROPANOLS
US4165384A (en) * 1974-11-01 1979-08-21 Aktiebolaget Hassle Amide substituted phenoxy propanol amines
US4387103A (en) * 1980-11-28 1983-06-07 American Hospital Supply Corporation Method for treatment or prophylaxis of cardiac disorders
US4471127A (en) * 1981-09-08 1984-09-11 Ciba-Geigy Corporation 1-5-Bis-(1,4-benzodioxin-2-yl)-3-azapentane-1,5-diols
US5039801A (en) * 1985-12-20 1991-08-13 The United States Of America As Represented By The Department Of Health & Human Services Thermal fragmentation of methylbenzylurea disastereomers or secondary amines and preparation of optically active secondary amines
JPS6364630U (en) * 1986-10-17 1988-04-28

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AT304474B (en) 1973-01-10
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DK140281C (en) 1979-12-10
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PL90038B1 (en) 1976-12-31
CH536813A (en) 1973-06-29
BG19132A3 (en) 1975-04-30
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CH536809A (en) 1973-06-29
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