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Pharmaceutical Substances Syntheses, Patents, Applications - Part 92 ppt

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alternative synthesis by reaction of 2-diethylan~inoethyl chloridc with 7-chloro-5-2-fluoropheny1-2-oxo-2,3- dihydro-1 H- l,4-benzodiazepine: GB 1 O4O 548 Roche; appl.. alternative synt

Trang 1

Flurbiprofen F 91 1

Flurazeporn

Reference(s):

US 3 567 710 (Hoffmann-La Roche; 2.3.1971; prior 3.6.1968)

alternative synthesis by reaction of 2-diethylan~inoethyl chloridc with 7-chloro-5-(2-fluoropheny1)-2-oxo-2,3-

dihydro-1 H- l,4-benzodiazepine:

GB 1 O4O 548 (Roche; appl 1.3.1963; USA-prior 2.3.1962)

Formulation(s): cps 1 0 mg, 15 mg; tabl 27.42 mg (as base); cps 15 mg, 30 mg; tabl 30 mg (as

monohydrochloride); cps 15 mg, 30 mg; s r cps 20 mg (as dihydrochloride)

Trade Narne(s):

D: Dalmadorm (Roche) Felison ( ~ a ~ r o ~ h & n ) J: Benozil (Kyowa)

Flurazepam 15130 Riker Flunox (Boehringcr Dalmate (Nippon Roche)

Staurodorm Neu Mldorm A.R (Piarn) USA: Dalmane (Rochc)

I: Dalmadorm (Roche) Valdorm (Valeas)

Use: anti-inflammatory, analgesic RN: 5104-49-4 MF: ClsH13F0, MW: 244.27 EINECS: 225-827-6

LDsU: >385 mg/kg (M, i.v.); 640 m g k g (M, p.0.);

117 rngkg (R, p.0.);

10 mglkg (dog, p.0.)

CN: 2-fluoro-a-methyl[l , 1'-biphenyl]-4-acetic acid

sodium salt

RN: 56767-76-1 MF: C,,H,,FNaO, MW: 266.25

bromobenzene 4'-brorno-3'- 4-acetyl-2-nitra- 4-ocetyC2-ornino-

Trang 2

912 F Flurbiprofen

A

HO''CH~

HzS04

COOH

0-CH,

0

4-ocetyl-2-fluoro-

biphenyl (1)

2-fluoro-4-biphe- nylylocetic ocid

ethyl 2-fluoro-4- biphenylylocetote (U)

1 NoOC,H,

2 H~c'O\

H3C O O CH3 2 dimethyl sulfotc

CH3

4-bromo-2-

fluorobiphenyl

2-(2-fluoro-4-biphenylyl)- 2-hydroxypropionic acid (111)

polyphosphoric acid

C H 2

2-(2-fluoro-4-bi- phenylyl)ocrylic acid

Reference ( s ) :

a DAS 1 518 528 (Boots; appl 19.1.1965; GB-prior 24.1.1964)

US 3 755 427 (Boots; 28.8.1973; GB-prior 24.1.1964)

US 3 793 457 (Adams Sectal; 19.2.1974; GB-prior 24.1.1964)

b GB 1 5 14 8 12 (Boots; appl 4.4.1975; valid from 31.3.1976)

similar method:

US 3 959 364 (Boots; 25.5.1976; GB-prior 24.5.1973)

alternative syntheses:

DOS 2 646 792 (Mitsubishi Petrochemical; appl 16.10.1976; J-prior 23.10.1975, 31.7.1976)

racemate resolution:

DOS 2 809 794 (Boots; appl 7.3.1978; GB-prior 8.3.1977, 18.1.1978)

Formulation(s): amp 50 mg; cps 200 mg; drg 50 mg, 100 mg; eye drops 0.3 mglml (as sodium salt

dihydrate); plaster 40 mg; s r cps 200 mg; suppos 100 mg; tabl 50 mg, 100 mg

Trade Name(s):

D: Froben (Kanoldt; 1980) Ocufen (Allergan) J: Froben (Kakenyaku)

Ocuflur (Pharm-Allergan) GB: Froben (Knoll; 1977) USA: Ocufen (Allergan; 1987)

F: Antadys (Theramex) Ocufen (Allergan)

Cebutid (Knoll; 1979) I: Froben (Boots Italia)

Trang 3

Flurotyl F 913

Flurotyl

(Flurothyl)

RN: 333-36-8 MF: C4H,F,0 MW: 182.06

LDs0: 46 mgkg (M, i.v.)

CN: 1,l'-oxybis[2,2,2-trifluoroethane]

No

F ~ ' O H -+ F ~ C - O N ~

2,2,2-trifluoro- (n)

ethanol (I)

Use: CNS stimulant convulsant

Reference(s):

US 3 363 006 (Pennwalt; 9.1 l968; prior 29.12.1955,20.6.1960)

Formulation(s): 2 ml in special inhalation device

Tmde Name(s):

USA: Indoklon (Ohio Med.);

wfm

Use: inhalation anesthetic

RN: 406-90-6 MF: C4H5F30 MW: 126.08 EINECS: 206-977-1

LD,,: 5600 mgkg (R, i.p.)

CN: (2,2,24rifluoroethoxy)ethene

ethanol (I)

montmorillonite 2 4 0 - 2 8 0 OC

ocetoldehyde

Reference(s):

a US 2 830 007 (Air Reduction Cornp.; 1958; appl 1953)

b US 2 870 21 8 (Air Reduction Cornp.; 1959; appl 1955)

Fonnulation(s): liquid for inhalation 125 rnl

Trang 4

914 F Fluspirilene

Trade Name(s):

USA: Fluorornar (Ohio Med.);

wfm

Use: neuroleptic KN: 1841 -19-6 MF: C,,H,,F,N,O MW: 475.58 EINECS: 217-418-6 LD,,: 106 mg/kg (M, i.m.);

>I46 mg/kg (R, i.m.)

CN: 8-[4,4-bis(4-fluorophenyl)butyl]-l-phenyl-l,3,8-triazaspiro[4.5]decan-4-one

NH2

1 -benzyl- aniline potassium

4-onilino- 1 -benzyl-

4-corbomoylpiperidine (I)

spiro[4.5]decane (11) 4,4-bis-(4-fiuaro-

phenyl)butyl bromide

Reference(s):

Fluspirilene

BE 633 914 (Janssen; appl 20.6.1963; USA-prior 22.6.1962)

US 3 238 216 (Jansscn; 1.3.1966; prior 22.6.1962, 20.6.1963)

DAS 1 470 125 (Janssen; appl 21.6.1963; USA-prior 22.6.1962)

Formulation(s): amp 1.5 mg10.75 ml, 2 mgl ml, 12 mg16 ml; vial 12 mg (2 mglml)

Trade Name(sJ:

D: Fluspi (Neuro Hexal) GR: Redeptin (Smith Klinc &

Kivat (Honnosan) USA: Imap (McNeil); wfm

Trang 5

Flutamide F 915

Use: antiandrogen, antineoplastic (hormonal)

RN: 133 11-84-7 MF: CllHl1F3N2O3 MW: 276.21 EINECS: 236-341-9

>2 glkg (dog, p.0.)

CN: 2-methyl-N-[4-nitro-3-(trifluoromethyl)phenyl]propanamide

Qc,

w

trifluoro-

msthylbenzene

1-nitro-3-tri- fluoromethyl- benzene

3-trifluoromethyl- aniline (I)

3'-trifluoromethyl- acetonilide

4-nitro-3-trilluoro

methylaniline (11)

isobutyryl

chloride (Ill)

Flutornide

pyridine

1 + UI d H 3 C ' ) ( 4 0 C F 3

C H , ~

3'-Lrifluorornethyl- isobutyronilide

Reference(s):

J Med Chem (JMCMAR) 10,93 (1967)

a DOS 2 130 450 (Scherico; appl 19.6.1971)

US 4 144 270 (Scherico; 13.3.1979; appl 26.6.1974)

b US 4 302 599 (Schering Co.; 24.11.1981; prior 10.9.1979)

synthesis of 4-nitro-3-trifluoromethylaniline:

Jones, R.G.: J Am Chem Soc (JACSAT) 69,2346 (1947)

medical use:

US 3 995 060 (Scherico; 30.11.1976; appl 11.9.1974)

US 4 139 638 (Schcring Corp.; 13.2.1979; appl 3.10.1977)

US 4 161 540 (Schering Corp.; 13.2.1979; appl 3.10.1977)

US 4 329 364 (Schering Corp.; 11.5.1982; appl 23.9.1976)

US 4 474 813 (Schering Corp 2.10.1984; appl 24.5.1982)

Formulation{s): cps 125 mg; tabl 250 mg

Trang 6

916 F Flutazolam

Trade Name(s):

D: Apimid (Apogepha)

Cytamid (esparma)

Flumid (Hexal)

Fluta GRY (GRY-Pharma)

Winthrop)

Fugerel (Essex Pharma; GR:

1984)

Flutazolam

Eulexine (Schering-Plough; J: Odyne (Nippon Kayaku)

Chimax (Chiron)

ATC: NOSBA Use: benzodiazepine anxiolytic, tranquilizer

RN: 27060-91-9 MF: CI9HIRC1FN2O3 MW: 376.82

LD,,,: 19 10 m g k g (M, p.0.);

>6 @kg (R, p.o.1

CN: 10-chloro- l l b-(2-fluoropheny1)-2,3,7,1 1b-tetrahydro-7-(2-h~droxyethyl)oxazolo[3,2-

d][l,4]benzodiazepin-6(5H)-one

2-amino-5-chloro- glycine ethyl estel

2'-fluorobenzo- hydrochloride

phenone

(cf flunitrozepom

synthesis)

U

o l ~ r n i n ~ m chloride

ethylene

oxide

Flutozolorn

u

7-chloro-5-(2- f1uorophenyl)- 1.3-dihydro-2H- 1,4-benzodioze- pin-2-one (I)

Rcference(s):

DOS 1 952 486 (Hoffmann-La Roche; appl 17.10.1969; USA-prior 18.10.1968)

synthesis of 7-chloro-5-(2-fluoropheny1)- 1,3-dihydro-2H- 1,4-henzodiazepin-2-one:

US 3 109 843 (Hoffinann-La Roche; 5.1 1.1963; prior 21.6.1962)

Formulation(s): tabl 4 mg

Trade Name(s):

J : Coreminal (Mitsui)

Trang 7

Fluticasone propionate F 9 17

Use: locally active glucocorticosteroid RN: 80474-14-2 MF: C,,H,,F,O,S MW: 500.58

CN: (6a,1 1j3,16a,17a)-6,9-Difluoro- l l-hydroxy-l6-methyl-3-oxo-l7-(1-oxopropoxy)androsta-1,4-diene-17-

carbothioic acid S-(fluoromethyl) ester

0

H,IO,, THF

-, 1

chloride

(cf diflucortolone

volerate)

2 H,S, DMF

q0*cH3 3 HCI H 2 0

~ ~ ~ C H , H0v-4

b - Me

or

1, arcl DMA, NaHC03

2 AgF CH&N

I1 . -,

F

Fluticasone propionate I

Reference(s):

BE 887 518 (Glaxo Group; appl 13.2.1981; GB-prior 15.2.1980)

L 109 656 (Chemagis LTD.;IL-prior 15.5.1994)

Phillipps, G.H et al.: 5 Med Chem (JMCMAR) 37,3717 (1994)

Formulation(s): aerosol for inh 44 pg, 110 pg, 220 pg; cream 0.05%; ointment 0.005%; nasal spray 0.05%

Trade Name(s):

D: Atemur (ASTA Medica Viani (Cascan; Glaxo I: Flixotide (Glaxo

Wellcome) GB: Cutivate (Glaxo Wellcome) USA: Cutivate (Glaxn Wellcome) Flutivate (Cascan; Glaxo Flixonase (Allen & Flonase (Glaxo Wellcome)

Flixotide (Allen &

Hanburys)

Trang 8

918 F Flutoprazepam

U s e : long a c t i n g b e n z o d i a z e p i n e anxiolytic

RN: 25967-29-7 MF: C,,H,,CIFN,O MW: 3 4 2 8 0

LD,,,: 2 1 1 0 mglkg (M, i.p.); 2 4 3 0 mgkg (M, p.0.);

2 2 3 0 mglkg (R, i.p.); 1 0 0 6 g/kg (R, p.0.);

I000 mgkg (rabbit, p.0.);

> I 0 glkg (dog, p.0.)

CN: 7 - c h l o r o - l -(cyclopropylmethyl)-5-(2-fluoropheny1)- 1 3 - d i h y d r o - 2 H - l , 4 - b e n z o d i a z e p i n - 2 - o n e

1 Brz

* 0 0

r

2-fluoro-

toluene

ethyl a-(2-fluoro-

benzyl)ocetoocetate

2 KOH

1 cyclopropylmethyl bromide

-,

LI

benzy1)-a-(4-chloro-

phenyloza)oceto-

ethyl 5-chloro-3-

(2-fluoropheny1)-

indole-2-corbo~ylote (11)

acetate (I)

propylrnethyl-3-

(2-fluoropheny1)-

indole-2-corbou-

I Flutoprozeporn

Trang 9

Flutrimazole F 919

CN 2 LiAIH,

CI

- CI -v

\ /

5-chloro-3- (2-fluoropheny1)- indole-2- carbonyl chloride

Referencefs):

DE 1 795 372 (Sumitomo; appl 20.9.1968; J-prior 22.9.1967)

DE 1 795 771 (Sumitomo; appl 20.9.1968; J-prior 2.1 1.1967)

US 3 925 364 (Sumitomo; 6.8.1974; appl 16.9.1968; J-prior 22.9.1967)

additional synthesis:

DOS 2 151 540 (Sumitomo; appl 15.10.1971; J-prior 17.10.1970)

DOS 2 113 122 (Sumitomo; appl 18.3.1971; J-prior 19.3.1970)

Formulation(s): tabl 2 mg

Trade Narnefs):

J : Restas (Banyu; 1985)

Flutrimazole

(UR-4056)

ATC: DOlA Use: topical antifungal RN: 119006-77-8 MF: C,,H,,F,N, MW: 346.38

CN: l-[(2-fluorophenyl)(4-fluorophenyl)phenylmethyl]-1H-imidazole

Trang 10

920 F Flutropium bromide

2.4'-difluoro-

benzophenone

(2-fluorophenyl)- Flutrimazole (4-fluoropheny1)-

phenylchloro- methane

Refewnce(s):

EP 352 352 (J Uriach &Cia.; appl 31.1.1990; prior 28.7.1988)

Formulation(s): cream 1 %

Trade Name(s):

E: Micetal (Uriach)

Flutropium bromide

ATC: R03BB Use: anticholinergic, bronchodilator RN: 635 16-07-4 MF: C,H,,BrFNO, MW: 478.40

LD,,: 53 m g k g (M, i.p.1; 11 m g k g (M, i.v.); 760 mgikg (M, p.0.); 228 mglkg (M, LC.);

77 mglkg (R, i.p.); 12.5 mglkg (R, i.v.); 740 m g k g (R, p.0.); 615 mgikg (R, s.c.)

CN: (endo,syn)-8-(2-fluoroethyl)-3-[(hydroxydiphenylacetyl)oxy]-8-methyl-8-azoniabicyclo[3.2.l]octane

bromide

1 PCI,

H

/ \ 2 N-carbobenzyloxynortropine

-

benzilate (Il)

I N a p J

2 H3C-Br

I1 -b *

nortropine benzilote bromide (N) 1 Flulropium bramide

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