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Pharmaceutical Substances Syntheses, Patents, Applications - Part 113 potx

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Ketamine K 1121 starting material: Kiihn, M.: J. Prakt. Chem. (JPCPAO) 156 (11), 103 (1940). b AT 198 263 (Synfarma; appl. 1955). Formulation(s): amp. 1 gl5 ml; cps. 250 mg Trade Name(s): D: Kebuzon (Steiner) Kentan-S (Sawai) Ketobutane (Yamagata) F: Ketazone (Beytout); wfm Ketazon (Kyowa) Ketobutazone (Sato; Toho) I: Chetopir (Sarm); wfm Ketazone (Kyowa Hakko) Ketophczon (Kissei) J: Hichillos (Kotani) Ketobutan (Santen) Vintop (Maruko) Ketamine ATC: NOlAX03 Use: analgesic, anesthetic RN: 6740-88-1 MF: C,3H,,C1N0 MW: 237.73 EINECS: 229-804-1 LD,,: 77 mgkg (M, i.v.) CN: (f)-2-(2-~hlorophenyI)-2-(methylamino)cyclohexanone monohydrochloride RN: 1867-66-9 MF: C,3H,,CIN0. HCI MW: 274.19 EINECS: 217-484-6 2-chloro- cyclopentyl- benzonitrilc magnesium bromide (2-chloro- benzoyl)- cyclopentone methylamine Reference(s): US 3 254 124 (Parke Davis; 31.5.1966; prior. 31.7.1961,29.6.1962). BE 634 208 (Parke Davis; appl. 27.6.1963; USA-prior. 29.6.1962). Formulation(s): amp. 50 mg/5 ml, 100 mg/2 ml, 500 mg/lO ml; inj. 5 mg/ml, 10 mglml, 25 mglml, 50 mglml (as hydrochloride) Trade Name(s): D: Ketanest (Parke Davis; as Kttamine Panpharma Ketalar (Parke Davis); wfm hydrochloride) (Panpharma; as Ketalar (Parke Davis; as Velonarcon (ASTA Medica hydrochloride) hydrochloride); wfm AWD; as hydrochloride) GB: Ketalar (Parke Davis) Ketaset (Bristol-Myers F: Kttalar (Parke Davis; as I: Ketalar (Parke Davis) Squibb; as hydrochloride); hydrochloride) J: Ketalar (Sankyo) wfm USA: Ketaject (Bristol); wfm 1122 K Ketanserin Ketanserin ATC: C02KDO1 Use: antihypertensive RN: 74050-98-9 MF: C,,H,,FN303 MW: 395.43 EINECS: 277-680-2 CN: 3-[2-[4-(4-fluorobenzoy1)- 1-piperidinyllethyll-2,4(1 H,3H)-quinazolinedione 1 -benzyl-4-cyano- 4-fluorophenyl- piperidine magnesium bromide ethyl chloro- formate (11) 0 ethyl anthranilate 1. S0Cl2 2. I11 chlaride 0 4-(4-fluarabenzoyl)- piperidine (111) 0 ethanol 0 3-(2-hydraxyethy1)- 2,4(1 H.3H)-quinozo- linedione (N) I Ketanserin I EP 13 612 (Janssen; appl. 7.1.1980; USA-prior. 8.1.1979, 12.10.1979). US 4 335 127 (Janssen; 15.6.1982; prior. 8.1.1979, 12.10.1979). alternative synthesis: EP-appl. 98 499 (Ravizza; appl. 27.6.1983; I-prior. 6.7.1982). Formulation(s): amp. 10 mg/2 ml, 50 mgllO ml; tabl. 20 mg, 40 mg Trade Natne(s): I: Perketan (Inverni della Serepress (Formenti) Beffa) Sufrexal (Janssen; 1987) Ketazolam K 1123 Ketazolam ATC: N05BA10 Use: tranquilizer RN: 27223-35-4 MF: C,,H,,CIN,O, MW: 368.82 EINECS: 248-346-3 LD,,: 2 gikg (M, p.0.); 5 gtkg (R, p.0.) CN: 1I-chloro-8,12b-dihydro-2,8-dimethyl-12b-phenyl-4H-[l,3]oxazino~3,2-d][l,4]benzodiazepine-4,7(6H)- dione 2. NHJ -+ CI bromide 2-amino-5- dimethyl 5-chloro-2- chlarobenzo- sulfate rnethylomino- phenone benzophenone diketene (11) L-2Ez-J Ketozolam "d= +" ' 11 / 0 H3C Referenceis): a US 3 575 965 (Upjohn; 20.4.1971; prior. 20.10.1969). b S~muskovicz, J. et al.: Tetrahedron Lett. (TELEAY) 1971,3665. DOS 1 947 226 (Upjohn; appl. 18.9.1969; USA-prior. 19.9.1968, 27.3.1969). Formulariort(s): cps. 15 mg, 30 mg, 45 mg Trade Name(s): D: Contamex (Beecham- GB: Anxon (Beecham); wfm Wiilfing); wfm I: Anseren (Novartis) 1124 K Ketobemidone Ketobemidone (Cetobemidone) ATC: N02ABOl Use: analgesic RN: 469-79-4 MF: C,SH2,N02 MW: 247.34 EINECS: 207-421-0 LD,,,: 14 mglkg (M, i.v.); 10 mgkg (R, i.v.) CN: 1-14-(3-hydroxy phenyl)-1-methyl-4-piperidiny1]-l-propanone hydrochloride RN: 5965-49- 1 MF: C,,H2,N02 . HCl MW: 283.80 0rMgACH3 + 1 1. sodium amide ethylmognesium 2. N.N-bis(2-chloro- bromide benzyl cyanide methaxypheny1)- 4-(3-methoxypheny1)- Ketobemidone 1 -methyl-4-propionyl- piperidine (I) Reference(s): DRP 752 755 (1. G. Farben; appl. 1942). alternative synthesis: Kiigi, H.; ~iescher, K.: Helv. Chim. Acta (HCACAV) 32,2489 (1949). Formulation(s): amp. 2 mg12 ml, 10 mg/lO ml, 50 mg150 ml; tabl. 5 mg (as hydrochloride) Trade Name(s): D: Cliradon (Ciba); wfm Ketoconazole ATC: DO 1AC08; GOlAF11; J02AB02 Use: antimycotic RN: 65277-42- 1 ME C2,H2,C12N404 MW: 53 1.44 EINECS: 265-667-4 LD,,: 32 mglkg (M, i.v.); 618 mgkg (M, p.0.); 86 mgkg (R, i.v.); 166 mglkg (R, p.0.); 23.3 mglkg (dog, i.v.); 178 mgkg (dog, p.0.) CN: cis- 1 -acetyl-4-[4-[[2-(2,4-dichloropheny1)-2-1 H-imidazol-1 -ylmethyl)- l,3-dioxolan-4- yl]methoxy]phenyl]piperazine Ketoprofen K 1125 2.4-dichloro- glycerol cis-2-(2,4-dichloro- *' imidozole phenacyl pheny1)-2-bromo- bromide methyl-4-hydroxy- methyl-1.3-dioxolane 1. NaOH 0 NaH I1 + __* sodium hydride OH 1 -ocetyl-4-(4- hydroxypheny1)- piperazine Ketoconazole I Reference (s): DOS 2 804 096 (Janssen; appl. 3 1.1.1978; USA-prior. 3 1.1.1977,21.11.1977). US 4 335 125 (Janssen; 15.6.1982; prior. 31.1.1977). Formulaiion(s): cream 20 mg/g (2 %); shampoo 2 %; sol. 20 mgiml; susp. 100mg; tabl. 200 mg Trade Name(s): D: Nizoral (Janssen-Cilag; Nizoral (Janssen-Cilag; I: Nizoral (Janssen; 1983) 1981) 1983) J: Nizoral (Kyowa Hakko) Terzolin (Janssen-Cilag) GB: Nizoral (Janssen-Cilag; USA: Nizoral (Janssen; 1981) F: KCtoderm (Janssen-Cilag) 1981) Ketoprofen ATC: M01AE03; M02AA10 Use: analgesic, anti-inflammatory RN: 2207 1-1 5-4 MF: C,,H,,O, MW: 254.29 EINECS: 244-759-8 LD,,: 500 mgkg (M, i.v.); 360 mgkg (M, p.0.); 350 mglkg (R, i.v.); 62.4 mglkg (R, p.0.) CN: 3-benzoyl-a-methylbenzeneacetic acid lysine saIt RN: 57469-78-0 MF: Cz2Hz8NzOs MW. 40.48 1126 K Ketorolac 3-methylbenzo- phenone 3-bromomethyl- benzophenone (3-benzoylphenyl)- diethyl carbonate acetonitrile (I) Reference(s): US 3 641 127 (Rh8ne-Poulenc; 8.2.1972; F-prior. 27.1.1967). DE 1 668 648 (Rhhe-Poulenc; appl. 26.1.1968; F-prior. 27.l.l967), methyl alternative syntheses: Ketoprofen DOS 2 646 792 (Mitsubishi Petrochemical; appl. 16.10.1976; J-prior. 23.lO.l975,31.7.1976). US 4 097 522 (Aziende Chim. Riun. Angelini Francesco; 27.6.1978; I-prior. 5.6.1975). ' DOS 2 744 832 (LEK; appl. 5.10.1977; YU-prior. 18.10.1976). DOS 2 744 833 (LEK; appl. 5.10.1977; YU-prior. 18.10.1976). DOS 2 744 834 (LEK; appl. 5.10.1977; YU-prior. 18.10.1976). iodide Formulation(s): cps. 50 mg, 100 mg; gel 2.5 %; s. r. cps. 200 mg, 320 mg (as lysine salt); suppos. 30.6 mg, 100 mg; vial 100 mg Trade Name(s): D: Alrheumun (Bayer Vital; 1975) Orudis (RhGne-Poulenc Rorer) F: Bi-Proftnid (Specia) KCtum (MCnarini) Profhid (Specia) Toprec (ThCraplix) GB: Ketocid (Trinity) Orudis (Rhhe-Poulenc Rorer) Oruvail (Rh8ne-Poulenc Rorer) Powergel (Searle) I: Artrosilene (Dompt; as lysine salt) Fastum (Menarini) Flexen (Lifepharma) Isok (San Carlo) Ketartrium (Esseti) Ketodol (Drug Research) Ketofen (Delsaz & Filippini; as lysine salt) Meprofen (AGIPS) Orudis (Rh8ne-Poulenc Rorer) Profend (Drug Research) Reuprofen (Terapeutico M.R.) Salient (Biomedica Foscama) Sinketol (Locatelli) J: Capisten (Kissei) Orudis (Hokuriku) USA: Orudis (Wyeth-Ayerst; 1977) Oruvail (Wyeth-Ayerst) Ketorolac ATC: MOlAB15; N02BE; SOlBCOS Use: non-steroidal anti-inflammatory, analgesic RN: 74103-06-3 MF: C,,H,,NO, MW: 255.27 LD,,,: 200 mglkg (M, p.0.) CN: (+)-5-benzoyl-2,3-dihydro-1H-pyrrolizine-l-carboxylic acid Ketorolac K 1127 tromethamine salt RN: 74103-07-4 MF: C,,H,,NO, . C4H,,N03 MW: 376.41 monosodium salt RN: 110618-38-7 MF: C,,H,,NNa03 MW: 277.26 succinimide benzamide chloride pyrrole (I) dimethyl sulfide 2-(methylthio)- pyrrole 5-benzoyl-2-(methyl- 6.6-dimethyl-5.7-dioxo- 1 -[2-(4.6-dioxo-2.2-dimethyl- thio)pyrrole (11) spiro[2.5]octone- 1,3-dioxon-5-yl)ethyl]-2- 4.8-dione (111) (rnethy1thio)-5-benzoylpyrrole (N) 2. HCI , CH OH J 1. 3-chloroperbenzoic acid 2. rnethonol 1 Ketoroloc I 1. KOH . CH30H 2. HCI 'f- dimethyl 5-benzoyl-1,2- dihydro-3H-pyrrolo[l,2-a]- pyrrole-l ,l -dicarboxylate (V) "W""?rCOOH 1. I11 , NOH 2. HCI CI 3. NaH 4. KOH. CH30H 5. HCI -, 0 Ho ocid benzoylpyrrole 1128 K Ketotifen ,?Yo , THF 0 . P0Cl3 IN-chloro- H benzmorpholide phosphoryl succinimide chloride 0 H 2-chloro- pyrrole 2-chloro-5- benzoylpyrrole (VI) I. NOH, DMF 1. NOH 2. KOH. CH,OH 2. HCI, CHPH 3. HCI VI + 111 b CH3 Reference(s): a,b US 4 347 186 (Syntex; 31.8.1982; appl. 20.10.1980). US 4 458 081 (Syntex; 3.7.1984; appl. 11.6.1982; prior. 20.10.1980). c US 4 873 340 (Syntex; 10.10.1989; appl. 29.5.1986). alternarive synthesis: DE 2 760 330 (Syntex; appl. 13.7.1977; USA-prior. 14.7.1976, 23.2.1977). DE 2 731 678 (Syntex; appl. 13.7.1977; USA-prior. 14.7.1976,23.2.1977). US 4 087 539 (Syntex; 5.2.1978; appl. 23.2.1977; prior. 14.7.1976). US 4 089 969 (Syntex; 16.5.1978; appl. 23.2.1977; prior. 14.7.1976; 23.2.1977). US 4 097 579 (Syntex; 27.6.1978; appl. 31.3.1977). Muchowski, J.M. et al.: J. Med. Chem. (JMCMAR) 28,1037 (1985). synthesis of enantiomers: EP 264 429 (Wisconsin Ala. Res. Found.; appl. 2.4.1987; USA-prior. 6.11.1986, 16.4.1986). Gazman, A. et al.: J. Med. Chem. (JMCMAR) 29,589 (1986). Formularion(s): amp. 10 mg, 15 mg, 30 mg; eye drops 0.5 %; suppos. 30 mg; tabl. 10 mg (as tromethamine salt) Trade Name(s): D: Acular (Pharm-Allergan) Toradol (Recordati; 1990) Toradol IM (Syntex; GB: Acular (Allergan) Toradol IM (Recordati; Roche; 1990) Toradol (Roche) 1990) I: Lixidol (Farmitalia) USA: Acular (Allergan) Ketotifen ATC: R06AX17; SOlGX08 Use: antiasthmatic, antihistaminic RN: 34580-13-7 MF: C,,H,,NOS MW: 309.43 EINECS: 252-099-7 LDso: 179 mglkg (M, p.0.) CN: 4,9-dihydro-4-(l-methyl-4-piperidinylidene)-1OH-henzo[4,5]cyclohepta[1,2-b]thiophen-l0-onc fumarate RN: 34580-14-8 MF: C,3H,N0,S MW: 425.51 Ketotifen K 1129 benzoyl peroxide KOH. CH30H -1 0 ti-bromosuccinimide 0 4-0x0-9.10-dihydro- 4H-benzo[4.5]cyclo- hepto[l.2-blthiophene (cf. pizotifen synthesis) , THF 1 -methylpiperidin- 0 0 4-ylmagnesium chloride 9- ond 10-bromo-4-0x0-4H- benzo[4.5]cyclohepta[1.2-blthiophene (I) seporotion over silica gel IV b 2N HCI ___, I Ketotifen 1 1130 K Khellin Reference(s): DAS 2 11 1 071 (Sandoz; appl. 9.3.1971; CH-prior. 11.3.1970, 31.7.1970). US 3 682 930 (Sandoz; 8.8.1972; CH-prior. I 1.3.1970,3 1.7.1970). DOS 2 144 490 (Sandoz; appl. 6.9.197 1; CH-prior. 24.9.1970,4.2.1971). US 3 749 786 (Sandoz; 8.8.1972; CW-prior. 11.3.1970). alternative syntheses: DOS 2 302 970 (Sandoz; appl. 22.1.1973; CH-prior. 24.1.1972). US 3 960 894 (Sandoz; 1.6.1976; CH-prior. 21.1.1972). US 4 128 549 (Sandoz; 5.12.1978; prior. 19.1.1973, 26.7.1974, 27.2.1976,3.2.1977). medical use as antiasthmatic: US 4 073 915 (Sandoz; 14.2.1978; CH-prior. 20.5.1975). Formulation(s): cps. 1 mg; syrup 0.02 %; tabl. 1 mg, 2 mg (as fumarate) Trade Name(s): D: Airvitess (Farmasan) generics Zadi ten (Sandoz) Astifat (Fatol) F: Zaditen (Novartis; 1980) J: Zaditen (Sandoz-Sankyo; Zaditen (Novartis Pharma; GB: Zaditen (Novartis; 1979) 1983) 1979) I: Allerkif (Edmond) Zatofug (Wolff) Totifen (Master Pharma) Khellin ATC: M03 Use: vasodilator RN: 82-02-0 MF: C,,H,,O, MW: 260.25 EINECS: 201-392-8 LDs,,: 30.6 mglkg (M, i.v.); 50.8 mglkg (M, p.0.); 34.4 mglkg (R, i.v.); 68.8 mglkg (R, p.0.) CN: 4,9-dimethoxy-7-methyl-5H-furo[3,2-g][1]benzopyran-5-one I Khellin Isolation from ethanolic extracts of fruits of Umbellifera Ammi visnaga. Reference(s): Spath, E.; Gruber, W.: Ber. Dtsch. Chem. Ges. (BDCGAS) 71, 106 (1938). Abu-Shady, H.; Soine, T.O.: J. Am. Pharm. Assoc. (JPHAA3) 41,481 (1952). total syntheses: Baxter, R.H. et al.: J. Chem. Soc. (JCSOA9) 1949,30. Clarke, J.R.; Robertson, A.: J. Am. Chem. Soc. (JACSAT) 71, 362 (1949). Clarke, J.R.; Robertson, A,: J. Chem. Soc. (JCSOA9) 1949,302. Geissman, T.A.; Halsall, T.G.: J. Am. Chem. Soc. (JACSAT) 73, 1280 (1951). Formulation(s): cps. 10 mg, 12 mg; drg. 1.25 mg, 10 mg; drops 50 mgl100 ml; ointment 0.1 g1100 g, 0.01 g1100 g; sol. 0.025 gll00 ml; suppos. 2.5 mg, 5 mg; tabl. 25 mg . sulfide 2-( methylthio )- pyrrole 5-benzoyl- 2-( methyl- 6.6-dimethyl-5.7-dioxo- 1 -[ 2-( 4.6-dioxo-2.2-dimethyl- thio)pyrrole (11) spiro[2.5]octone- 1,3-dioxon-5-yl)ethyl ]-2 - 4.8-dione (111). cis- 1 -acetyl- 4-[ 4-[ [ 2-( 2,4-dichloropheny1 )-2 -1 H-imidazol-1 -ylmethyl )- l,3-dioxolan- 4- yl]methoxy]phenyl]piperazine Ketoprofen K 1125 2.4-dichloro- glycerol cis- 2-( 2,4-dichloro- *'. RN: 7405 0-9 8-9 MF: C,,H,,FN303 MW: 395.43 EINECS: 27 7-6 8 0-2 CN: 3-[ 2-[ 4-( 4-fluorobenzoy1 )- 1-piperidinyllethyll-2,4(1 H,3H)-quinazolinedione 1 -benzyl-4-cyano- 4-fluorophenyl- piperidine

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