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Pharmaceutical Substances Syntheses, Patents, Applications - Part 150 pps

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Opipramol 0 1491 Trade Name(s): D: Zofran (Glaxo Wellcome) GB: Zofran (Glaxo Wellcome; J: Zofran (Glaxo-Sankyo, F: Zophren (Glaxo Wellcome) 199 1) Sankyo) I: Zofran (Glaxo Wellcome) USA: Zofran (Glaxo Wellcome) Opipramol ATC: N06AA05 Use: thymoleptic, antidepressant RN: 315-72-0 MF: C2,H2,N30 MW: 363.51 EINECS: 206-254-0 LD,,,: 45 mglkg (M, i.v.); 400 mglkg (M, p.0.); 32 mgkg (R, i.v.); l I1 0 mglkg (R, p.0.) CN: 4-[3-(5H-dibenz[b,flazepin-5-yl)propyl]- 1 -piperazineethanol dihydrochloride RN: 909-39-7 MF: C2,H2,N30 . 2HCl MW: 436.43 EINECS: 213-000-2 LD,,: 45 mgkg (M, i.v.); 443 mglkg (M, p.0.); 32 mgkg (R, i.v.); 900 mglkg (R, p.0.) -1- - ,. 1. sodium amide 2. 1 -brorno-3-chloro- 5H-dibenz[b,f]ozepine propane 5-(3-chlorapropyl)-5H- dibenz[b.f]azepine (I) 2-piperozinoethonol ( Opiprornol Reference(s): GB 862 297 (Geigy; appl. 8.5.1958; CH-prior. 9.5.1957). FR 1 271 971 (Geigy; appl. 12.8.1959; CH-prior. 13.8.1958). GB 881 398 (Rh6ne-Poulenc, appl. 29.9.1958; valid from 7.9.1959). DE 1 132 556 (Geigy; appl. 12.8.1959; CH-prior. 13.8.1958). DE 1 133 729 (Geigy; appl. 8.5.1958; CH-prior. 9.5.1957). Formulation(s): drg. 50 mg (as dihydrochloride) Trade Name(s): D: lnsidon (Novartis Pharma) I: Insidon (Novartis Farma) F: Insidon (Novartis) J: Insidon (Geigy-Fujisawa) GB: lnsidon (Geigy); wfm USA: Ensidon (Ciba-Geigy); wfm Orazamide (AICA-Orotate) ATC: A05B Use: liver therapeutic RN: 2574-78-9 MF: C5H4N,04. C,HdN40 MW: 282.22 EINECS: 219-923-7 LD,,,: 600 mglkg (M, i.p.) CN: 5-amino-1 H-imidazole-4-carboxamide orotate (1 : 1) 1492 0 Orciprenaline 0 H H ON0 OH ON0 \ NH HzN 0 ONa HzN COOH Refereme(s): GB 1 018 117 (Fujisawa; appl. 13.3.1963; J-prior. 15.3.1962). US 3 271 398 (Fujisawa; 6.9.1966; J-prior. 15.3.1962). 4-orninoirnidozole-5- sodium orotote corboxomide newer method for AICA: DE 2 160 674 (Sagami; appl. 29 .l2.1971; J-prior. 9.12.1970). Orozornide Formulation(s): tabl. 100 mg hydrochloride Trade Name(s): D: Aicorat (Mack, Illert.); F: Aicamine (Labaz); wfm J: Aicamin (Fujisawa) wfm I: Aicamin (Crinos); wfm Orciprenaline (Metaproterenol) ATC: R03AB03; R03CB03 Use: bronchodilator, antiasthmatic RN: 586-06-1 MF: C,,H,,NO, MW: 211.26 EINECS: 209-569-1 LDs,,: 86 mglkg (M, i.v.); >8130 mgkg (M, p.0.); 67.2 mgkg (R, i.v.); 3370 mgkg (R, p.0.); 30 mgkg (dog, i.v.); 125 mglkg (dog, p.0.) CN: 5-[1-hydroxy-2-[(1-methylethyl)amino]ethyl]-1,3-benzenediol sulfate (2:l) RN: 5874-97-5 MF: CllHI7NO3 1/2H2S04 MW: 520.60 EINECS: 227-539-6 LD,,: 114 mglkg (M, i.v.); 4800 mglkg (M, p.0.); 5538 mgkg (R, p.0.) 0 CH, K 0 0 CH, K 0 3',5'-diocetoxyoceto- 2-brorno-3',5'-di- phenone ocetoxyocetophenone + 11 1. isopropylornine (1) 3',5'-dihydroxy- 2-(isopropylornino)- ocetophenone (11) Orciprenoline u Orgotein 0 1493 3',5'-dirnethoxyaceto- 2-brorno-Y.5'-di- 2-iropropylarnino-3',5'-di- phenone rnethoxyacetophenone rnethoxyocetophenone (III) HBr H2, Raney-Ni 111 r 11 Reference(s): DE 1 275 069 (Boehringer Ing.; appl. 15.2.1960). US 3 341 594 (Boehringer lng.; 12.9.1967; D-prior. 15.2.1960). Formularion(s): amp. 0.5 mg; doses aerosol 1.5 mg, 0.75 mg; drops 2 %; inhalation aerosol 750 pghetered inhalation; syrup 10 mg/5 ml; sol. 15 mg; tabl. 20 mg (as sulfate) Trade Name(s): D: Alupent (Boehringer Ing.) I: Alupent (Boehringer Ing.) USA: Alupent (Boehringer Ing.) F: Alupent (Boehringer Ing.) J: Alotec (Boehringer- generics GB: Alupent (Boehringer Ing.) Tanabe) Orgotein ATC: MOIAX14 Use: anti-inflammatory RN: 9054-89- 1 MF: unspecified MW: unspecified EINECS: 232-771-6 CN: dismutase superoxide Water soluble protein with a relative molecular mass of ca. 32600, which particularly contains copper and zinc bound like chelate (ca. 4 gram atoms) and has superoxide-dismutase-activity. It is isolated from bovine liver or from hemolyzed, plasma free erythrocytes obtained from bovine blood. Purification by manyfold fractionated precipitation and solvolyse methods and definitive separation of the residual foreign proteins by denaturizing heating of the orgotein concentrate in buffer solution to ca. 65-70 "C and gel filtration andlor dialysis. Reference(s): DE 2 101 866 (Diagnostic Data; appl. 15.1.1971; USA-prior. 16.1.1970). US 3 579 495 (Diagnostic Data; 18.5.1971 ; prior. 13.5.1968, 10.4.1969, 24.4.1970). US 3 624 251 (Diagnostic Data; 30.1 1.1971; appl. 16.1.1970). US 3 687 927 (Diagnostic Data; 29.8.1972; prior. 31.8.1966, 2.8.1967,7.6.1971). Formulation(s): vial 4 mg, 8 mg Trade Name(s): D: Peroxinorm (Griinenthal); Interceptor (Isnardi); wfm Oxinorm (Zambeletti); wfm Orgo-M (Max Farma); wfm wfm I: Artrolasi (Ausonia); wfm Orgoten (Serono); wfm 1494 0 Orlistat Orlistat ATC: A08AB01 (Tetrahydrolipstatin; Orlipastat; Ro- 18-0647) Use: antiobesity, pancreatic lipase inhibitor RN: 96829-58-2 MF: C2,Hs3NOs MW: 495.75 CN: N-Formyl-t-leucine [2S-[2a(R*),3.beta.]]-l-[[3-hexyl-4-oxo-2-oxetanyl]methyl]dodecyl ester I CHO \CHO lipstatin Orlistat lipstotin is produced by fermentation ol Streptornyces toxytricini ethyl 3(R)-(tetrohydro- pyranyloxy)-6-heptenoate "' p I, THF, Et.0 H3C-(CH2)6-p+ 2. BuLi I + - 2. butyllithiurn octyltriphenylphosphoniurn bromide DIBAL. toluene. CH~C~~ fu 11 0 0 b N diisob~t~lalurninum 0HCh(CH2)6-CH3 octanoic acid (nI), hydride butyllithium. diisopropylamide 9. ,Cl l.Qf,; , pyridine z.To-O* . . C~H,OH 3. separation of diastereomers A l OH 0 0 by column chromatorophy HOOC-(cH,),- CH, b v 1. benzenesulfonyl chloride (CH2),-CH, 2. pyridinium p-toluenesulfonate mixture of diastereorners Orlistat 0 1495 1. PPh3. DEAD. THF + - Orlistot HN,CHO 1. triphenylphosphine HO (S)-N-formyl- leucine (VI) 1. CH2C12, cyclohexone NH toluene. CH,CI,. -78T + CI3CAO"$ b VIlI 2. LiH-DIBAL methyl (R)-3-hydroxy- benzyl trichloro- tetrodeconoote ocetimidote (VII) 1. KOH. CH,OH ______, 1. potossium hydroxide 2. benzenesulfonyl (XI chloride 1. Hz, Pd-C, THF 2. V . PPh,, DEAD. THF b Orlistat 2. (S)-N-formylleucine (XI) (-)-N-methyl- octonoyl chloride ephedrine 1496 0 Orlistat YHa 2. CI-5'-CH3 XI1 CH3 t M 1. butyllithiurn, diisopropylarnine 2. trirnethylsilyl chloride QH + J'J "3 . ""2 , 0 HOOC~COOH o boron H 00 C,,+\\~O L' trifluoride 0 etherote (S)-rnolic acid cyclo- (w hexonone 1. BH THF 1. BH3, THF 2. CI-SiPh tBu 2. 2 , tBuPh Si OH - - Xlll 'c 1-7k0'CH b XIV 3 1. borone 1. borone 0 2. tert-butyl- 2. 2-naphthylsulfonyl diphenylsilyl chloride chloride 1. Li-(CHZ)9-CH, 2. VI1 XV , tBuPh Si 1. decyllithium 'o-(cH~)~~- CH3 2. benzyl trichloroocetirnidote (W 1. HF. CH3CN 2. Py2 . H,Cr,O, '1- OHC- 2. pyridinium (CH2) ,0- CH3 dichrornote 3(R)-benzyloxy- tetrodeconol (XVII) Orlistat 0 1497 the diastereomers are separated by column chromotogrophy 1. HF, CH,CN ?p 1. CI-Tbs 2. 03 ,.a\; .O 3. NaC102 Tbs\o 3. separation XVUI H00c+(~~2)lo- CH~ -xx (CH2),-CH3 1. Hz. Pd-C 2.VI. PPh,. DEAD m, Orlistat 2. (S)-forrnylleucine, triphenylphosphine finalization of synthesis from the stereoisomer XDC 1. CI-Tbs 1. HF. CH,CN 2. 0, 3. NaC102 Tbs, '"8 2.Tos-Cl, 0 m - ~ooc& + XI (CH2) 1,- CH3 1. Hz. Pd-C 2. VI , PPh,. DEAD XI _______* Orlistot olternotive synthesis of 3(R)-benzyloxytetradecanal XM THF OH 0HC-(CH2)g-CH3 + H2C'kM'@r -+ H2~/d(~~2) ,,- CH3 allylmagnesium bramide 1498 0 Orlistat Z(R)-ocetoxy-2- phenylocetic ocid 1. KOH. CH,OH (m) (XXIII) the diastereomers are separoted by column chromatography 2. benzyl bromide (XXUI) H~C'M(CH,),~- CH, 1. KOH. CH,OH ~.O~N-(~COOH. PP~,. DEAD. K~CO, b OH isomerization of unwonted stereoisomer H~c/~(cH,)~~- CH, 1. XXN. KH, THF 2. 0,. cn30H. CH~CI~ , XVII 1. benzyl bromide 2. ozone LDA, THF OH OH XVII + 111 H~~~+(cH,)~~- CH, lithium diiso~ro~vl- (CH,),-CH, . ., omide (mu mixture of diastereomers 1. Hz. Pd-C.THF 2. Tos-OH, CHCI, H,C XXYI + , XXVlll (Jones oxidation) (mI0 mixture of diastereorners Orlistat 0 1499 1. XXIII, THF, HMPT A 2.0, To ,, CH2Cl, xx)[I b o Yn o o 1. benzyl bromide H~~~~(cH~)~~-cH~ 2. 3.4-dihydro-2H-pyron (IOWI) (EH,),-CH, (mu) 's'~' 1 ,\ . pyridine 1. benzenesulfonyl chloride 2. pyridiniurn p-toluenesultonote PPh,. DEAD Orlistot CH 2. DIBAL, toluene ~~cK~~(CH ) - CHI + xm b vrrr 2 10 2. diisobutylalurninurn tert-butyl (R)-3-hydroxy- tetradeconoote hydride THF, -7B°C tert-butyl (S)-p-toluene- sulfinylocetate 1. Hg-AI. THF, H20 2. Br-(CH2),-CH, , BuLi, 2. hexyl bromide, butyllithium (CHJ-CH, 1. KOH, CH,OH - - 1500 0 Orlistat 2. VI. PPh3. DEAD, THF XXXYII Orlistat (3 0 OH pyridine H C \~~(w~),~-cH~ methyl (R)-3-hydroxy- a-bromooctanoyl tetradeconoate (XXXVIII) chloride a-bramooctanoic acid 7% Zn. Et,O, CI-~~-CH, XXW( '3'3 + XW( d Orlistat zinc, trirnethyl- silyl chloride analogously to method Reference(s): a EP 129 748 (Hoffmann-La Roche & Co. AG; appl. 2.1.1985; CH-prior. 22.6.1983). b Schneider, F.; Barbier, P.: Helv. Chim. Acta (HCACAV) 70,196 (1987). synthesis uf3(R)-(tetrahydropyrany1oxy)-6-heptenc acid ethyl ester: Hirama, M.; Nei, M.: J. Am. Chem. Soc. (JACSAT) 104,4251 (1982). c Widmer, U.; Schneider, F.; Barbier, P.: Helv. Chim. Acta (HCACAV) 70,1412 (1987). d Hanessian, S.; Tehim, A,; Chen., P.: J. Org. Chem. (JOCEAH) 58 (27), 7768 (1993). e Barbier, P.; Schneider, F.: J. Org. Chem. (JOCEAH) 53, 1218 (1988). f EP 189 577 (Hoffmann-La Roche & Co. AG; appl. 6.8.1986; CH-prior. 21.12.1984). g EP 524 495 (Hoffmann-La Roche & Co. AG; appl. 27.1.1993; USA-prior. 23.7.1991; 12.3.1992). ,further synrheses of orlistat: Kocieski, P.; Pons, J.M.: Tetrahedron Lett. (TELEAY) 30, 1833 (1989). Fleming, I.; Lawrence, N.J.: Tetrahedron Lett. (TELEAY) 31 (25), 3645 (1990). Casc-Green, S.C.; Davies, S.G.; Hedgecock, C.J.R.: Synlett (SYNLES) 1991,781 Uskovic, M.R.; Chadka, N.K.; Batcho, A.D.; Tang P.C.; Courtney, L.F.; Cook C.M.; Wovliulich, P.M.: J. Org. Chem. (JOCEAH) 56,4714 (1991). Formulation(s): cps. 120 mg Trade Nume(s): D: Xenical (Roche; 1999) GB: Xenical (Roche; 1998) F: Xenical (Roche; 1998) USA: Xenical (Roche; 1998) . antiobesity, pancreatic lipase inhibitor RN: 9682 9-5 8-2 MF: C2,Hs3NOs MW: 495.75 CN: N-Formyl-t-leucine [2S-[2a(R*),3.beta.]]-l-[[3-hexyl-4-oxo-2-oxetanyl]methyl]dodecyl ester I CHO CHO lipstatin. 1493 3',5'-dirnethoxyaceto- 2-brorno-Y.5'-di- 2-iropropylarnino-3',5'-di- phenone rnethoxyacetophenone rnethoxyocetophenone (III) HBr H2, Raney-Ni 111 r 11 Reference(s):. 125 mglkg (dog, p.0.) CN: 5-[ 1-hydroxy- 2-[ (1-methylethyl)amino]ethyl ]-1 ,3-benzenediol sulfate (2:l) RN: 587 4-9 7-5 MF: CllHI7NO3 1/2H2S04 MW: 520.60 EINECS: 22 7-5 3 9-6 LD,,: 114 mglkg (M, i.v.);

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