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Pharmaceutical Substances Syntheses, Patents, Applications - Part 221 potx

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tert-butyl hypobromite H3C,C-0-Br tert-butyl methoxy-3-phenyl- propane UI... sodium hyposulfite Ziprasidone hydrochloride u... tin1l chloride S-4-4-hydrozinobenzy1- 2-oxozolidinon

Trang 1

Zipeprol Z 2201

Zimeldine

2 134 379 (AB HBssle; appl 12.4.1972; S-prior 28.4.1971)

alternative syntheses:

BE 835 802 (Astra; appl 21.1 1.1975; S-prior 21.1 1.1974)

SU 650 501 (Pharmastra; appl 21.5.1976)

Formulation(s): 100 mg, 200 mg (as dihydrochloride)

Trade Name(s):

D: Normud (Astra); wfm GB: Zelmid (Astra); wfm

Use: antitussive RN: 34758-83-3 MF: CZ3H3,N,O3 MW: 384.52 EINECS: 252-191-7

CN: 4-(2-methoxy-2-phenylethyl)-a-(methoxyphenylmethyl)-1-piperazineethanol

dihydrochloride

RN: 34758-84-4 MF: C2,H3,NzO3 2HCl MW: 457.44 EINECS: 252-192-2

LD,,: 44.3 mglkg (M, i.v.); 300 mglkg (M, p.0.);

32.7 mglkg (R, i.v.); 435 mglkg (R, p.0.);

228 mglkg (dog, p.0.)

tert-butyl hypobromite

(H3C),C-0-Br

tert-butyl

methoxy-3-phenyl- propane (UI)

Trang 2

2202 Z Ziprasidone hydrochloride

Rejerence(s):

US 3 7 18 650 (Mauvernay; 27.2.1973; F-prior 2.3.1970)

DE 2 109 366 (CERM; appl 30.9.1971; prior 27.2.1971)

Formulation(s): drg 75 mg; syrup 0.5 % (as dihydrochloride)

Trade Name(s):

F: Respilhe (Winthrop; 1973) I: Zitoxil (Italfarmaco; 1979)

Ziprasidone hydrochloride

(CP-88059-1)

Use: antipsychotic, dopamine D2- antagonist, 5-HT2-antagonist

RN: 138982-67-9 MF: C21H2,ClN40S HCl H 2 0 MW: 467.42

CN: ~-[2-[4-(l,2-Benzisothiazol-3-yl)-l-piperazinyl]ethyl]-6-chloro-l,3-dihydro-2H-indol-2-one

hydrochloride hydrate

base

RN: 146939-27-7 MF: CzIH2,ClN4OS MW: 412.95

hydrochloride

RN: 122883-93-6 MF: C,IH21ClN40S~ HCl MW: 449.41

mesyIate

RN: 18.5021-64-1 MF: C21H21ClN40S CH403S MW: 509.05

chloroocetyl chloride

0

H,c,;~,cH, '

H CF,COOH

c I , u triethylsilane,

trifluoroacetic

(2-chloroethy1)- oxindole (n)

Trang 3

Ziprasidone hydrochloride Z 2203

I-(1,2-benziso-

thiazol-3-yl)-

piperozine (111)

1 POCI,

(\NH

2 ~ ~ 3

2 piperazine

2.5-dichloro-

taluene

Ziprasidone hydrochloride

I

H3c-C~CH, H3C-N,

CH, CH3

THF

,

tert-butoxybis-

rnethone

Xo2 H3C CH3COOH PN CI CH,COOH C I / ' V ~ '

IV + Ill - S,N, N , -+ V

borohydride

1 3 N HCI

2 SOCI2, C Y O H

3 No2Sp04, THF H 2 0

VI - 3 sodium hyposulfite

Ziprasidone hydrochloride

u

Trang 4

2204 Zolimidine

Reference(s):

a Howard, H.R et al.: J Labelled Compd Radiopharm (JLCRD4), 1994, 51

US 5 206 366 (Pfizer; 27.4.1993; USA-prior 26.8.1992)

EP 281 309 (Pfizer; appl 24.2.1988; WO-prior 2.3.1987)

b Urban, F.J et al: Synth Commun (SYNCAV) 26 (a), 1629-1638 (1996)

IJS 5 359 068 (Pfizer; 25.10.1994; USA-prior 28.6.1993)

monohydrate:

EP 586 191 (Pfizer; appl 25.8.1993; USA-prior 1.9.1992)

mesylate dihydrate salts:

WO 9 742 191 (Pfizer; appl 10.4.1997; USA-prior 7.5.1996)

cyclodextrin inclusion complexes:

EP 81 1 386 (Pfizer; appl 24.4.1997; USA-prior 7.5.1996)

Formulation(s): cps 20 mg, 40 mg, 60 mg, 80 mg

Trade Name(s):

USA: Zeldox (Pfizer)

Use: ulcer therapeutic RN: 1222-57-7 MF: C,4H,2N202S MW: 272.33 EINECS: 214-947-4

LD,,,: >4 glkg (M, p.0.);

3710 mglkg (R, p.0.)

CN: 2-[4-(methylsulfonyl)phenyl]imidazo[1,2-a]pyridine

I Zolirnidine

Refererzce(s):

GB 991 589 (Lab Bioterapico Milanese Selvi; valid from 23.7.1963; I-prior 30.4.1963)

Almirante, L et al.: J Med Chem (JMCMAR) 8, 305 (1965)

Formula~ion(s): cps 200 mg

Trade Narne(s):

1: Solimidin (Selvi); wfm USA: Mutil (Lakeside); wfm

Zolmitriptan

(31 1C90; BW-311C90)

ATC: N02CC03 Use: antimigraine agent, 5-HT,D-agonist RN: 139264-17-8 MF: C,,H2,N302 MW: 287.36

CN: (S)-4-[[3-[2-(dimethylamino)ethyl]-1H-indol-5-yl]methyl]-2-oxazolidinone

monohydrochloride

RN: 139264-19-0 MF: C,6H2,N302 HCl MW: 323.82

racemic monohydrochloride

RN: 139346-15-9 MF: C,,H2,N302~ HCl MW: 323.82

Trang 5

Zolmitriptan Z 2205

synthesis of intermediote 111:

1 S0CI2 CH,OH

HOOC

2 sodium borohydride

4-nitro-L-phenyl-

olonine (I)

1 KOH or NoOH

2 H2, Pd-C

3 NaN02 HCI

0 4 SnCI2 0 H

n + CI ,,l 0 /CCI3 - 2 hydrogen pollodium

3 sodium nitrite di~hosgene 4 tin(1l) chloride (S)-4-(4-hydrozinobenzy1)-

2-oxozolidinone hydrochloride (Ill)

or:

1 KOH or NoOH

2 H2 Pd-C

3 NoNO,, HCI

4 SnClp

2 hydrogen pollod~um

3 sodium nitrite phosgene

4 tin(l1) chloride

synthesis of intermediote V:

1 H20, KOH 0

2 Hz, Pd-C

2 hydrogen

pallodium benzyl

isocyanote

1 NoN02 HCI 0

2 SnCI, H

N 1 sodium nitrite ,

2 tin@) chloride '

(5)-5-(4-hydrozinobenzy1)-

2.4-imidozolidinedione hydrochloride (V)

butonol diethyl

ocetal (VI)

I

Trang 6

2206 Z Zolmitriptan

1 C2H50H, H20, A

2 H2C=0 H20 CH30H

3 NoCNBH3

4 FH3

111 +

2 formaldehyde

3 sodium cyonoborohydride 4-chlorabutanol 4 dimethylomine (WI)

diethyl ocetal (VII)

3-cyonoproponol

diethyl ocetal

1 PPE, CHC13, A

2 Hz Pd-C C2H50H VIIl

D

1 polyphosphote ester

2 hydrogen, pollodium, ethanol

1 C2H50H H20 A

2 Bo(OH), H20

v + V I - 2 borium hydroxide

HOOC

N-CH3 H3C

3-[3-(2-dimethylominoethyl)- 1H-indol-5-yl]-L-alanine (X)

2 sodium barahydride

3 diethyl carbonate, potassium

carbonote

alternative synthesis of X:

1 C2H50H H20 A

2 HzC=O H20 CH,OH

3 NoCNBH3

4 VIII

5 BO(OH)~, H20

v + vn b x

3 sodium cyonoborohydride

5 borium hydroxide

Reference(s):

WO 9 1 18 897 (The Wellcome Foundation; appl 12.12.1991; GB-prior 7.6.1990, 1.2.1991) Glenn, R.C et al.: J Med Chem (JMCMAR) 38,3566 (1995)

Trang 7

Zolpidem Z 2207

synthesis of 4-dimethylaminobutanal diethyl acetal:

Desaty, K.: Croat Chem Acta (CCACAA) 36, 103, 107 (1964)

Somin, I.N et al.: J Org Chem (JOCEAH) 1,201 1 (1965)

Bhattacharyya, S.: Tetrahedron Lett (TELEAY) 35 (IS), 2401 (1994)

Harries et al.: Justus Liebigs Ann Chem (JLACBF) 410,65 (1915)

synthesis of 4-chlorobutanal diethyl acetal:

Loftfield: J Am Chem Soc (JACSAT) 73, 1365 (1951)

Anet et a].: Aust J Sci Res Ser A (AJSRA2) 3, 336 (1950)

Winterfeld et al.: Arch Pharm Ber Dtsch Pharm Ges (APBDAJ) 293, 325 (1960)

Tamelen, Van et al.: Bioorg Chem (BOCMBM) 5,283 (1976)

Formulation(s): f c tabl 2.5 mg; tabl 2.5 mg

Trade Narne(s):

D: Asco Top (Zeneca) GB: Zomig (Zeneca)

Zolpidem

(SL-80-0750-23N)

ATC: N05CF02 Use: hypnotic with affinity to benzodiazepine receptor RN: 82626-48-0 MF: C,9H21N,0 MW: 307.40

CN: N,N,6-trimethyl-2-(4-methylphenyl)imidazo[1,2-a]pyridine-3-acetamide

tartrate (2:l)

RN: 99294-93-6 MF: C,,H2,N30 1/2C4H60, MW: 764.88

LD,,: 695 mg/kg (M, p.0.);

2700 m g k g (R, p.0.)

tartrate (1:l)

RN: 103188-50-7 MF: C,,H2,N,0 C4H,06 MW: 457.48

2-amino-5- bromomethyl 2-(4-methylpheny1)-6-

rnethylpyridine 4-methylphenyl methylimidozo[l -2-01-

ketone pyridine (I)

1 CH31

" 3 C

2 NoCN

r H3C

1 methyl iodide NC'

2 sodium cyonide

1 HCI, CH3COOH

2 P0Cl3

3 n

111 -b

2 phosphoryl

chloride

Trang 8

2208 Z Zomepirac

2.2-dimethoxy-

N.N-dimethyl-

ocetomide

Reference(s):

a EP 50 563 (Synthelabo; appl 15.10.1981; F-prior 22.10.1980)

DE 3 163 524 (Synthelabo; appl 15.10.198 1; F-prior 22.10.1980)

b EP 251 859 (Synthelabo; appl 17.6.1987; F-prior 27.6.1986)

2,2-dimethoxy-N,N-dimethylacetamide:

US 3 361 757 (Du Pont; 15.1 1.1965)

Formulation(s): f c tabl 10 mg; tabl 5 mg, 10 mg (as tartrate)

Trade Name(s):

D: Bikalm (Byk Gulden) Stilnox (SynthClabo; 1988) Stilnox (Synthelabo; 1990) Stilnox (Synthelabo) GB: Stilnoct (Lorex) J: Myslee (Fujisawa) F: Ivadal (Cipharm) I: Niotal (Synthelabo) USA: Ambien (Searle)

Use: analgesic, anti-inflammatory RN: 33369-31-2 MF: C,,H,,C1NO3 MW: 291.73 EINECS: 251-474-2

CN: 5-(4-chlorobenzoyl)- 1,4-dimethyl-1 H-pyrrole-Zacetic acid

sodium salt dihydrate

RN: 64092-49-5 MF: C,,H,,ClNNaO, 2H20 MW: 349.75

pyrrole-2-ocetote (I)

4-chlorobenzoyl

chloride

Trang 9

Zonisamide Z 2209

11

quinoline copper chrornite ' I 0 0 m4

Zomepirac

Reference(s):

DE 2 102 746 (McNeil; appl 21.1.197 1 ; USA-prior 26.1.1970)

US 3 952 012 (McNeil; 20.4.1976; prior 16.2.1973, 26.1.1970, 1.7.1968, 26.7.1967)

Carson, J.R.; Wong, S.: J Med Chem (JMCMAR) 16, 172 (1973)

alternative syntheses:

BE 762 060 (McNeil; appl 26.1.1971; USA-prior 26.1.1970)

DOS 2 339 140 (McNeil; appl 2.8.1973; USA-piior 3.8.1972)

US 3 865 840 (McNeil; 11.2.1975; prior 16.2.1973, 26.7.1967, 1.7.1968, 26.1.1970)

Formulation(s): tabl 100 mg (as sodium salt dihydrate)

Trade Name(s):

D: Zornax (Cilag); wfm F: Zomax (Cilag); wfm USA: Zomax (McNeil); wfm

RN: 68291-97-4 MF: CuH,N203S MW: 212.23

LD,: 699 rnglkg (M, i.p.); 816 mglkg (M, i.v.); 1829 mglkg (M, p.0.); 1009 mglkg (M, s.c.);

733 rnglkg (R, i.p.); 672 mglkg (R, i.v.); 1992 mglkg (R, p.0.); 925 mglkg (R, s.c.);

1 glkg (dog, p.0.)

CN: 1,2-benzisoxazole-3-methanesulfonamide

monosodium salt

RN: 68291-98-5 MF: CuH,N2Na0,S MW: 234.21

1 P0Cl3

"

- -No

"Br sulfite ->-u II

1,2-benzisoxozole (I) isoxazole-3-methane-

sulfonote

Reference(s):

DE 2 825 410 (Dainippon; appl 9.6.1978)

US 4 172 896 (Dainippon; 30.10.1979; appl 5.6.1978)

Uno, H et al.: J Med Chem (JMCMAR) 22, 180 (1979)

Trang 10

2210 Z Zopiclone

synthesis of3-bromomethyl-1,2-benzisoxazole:

Uno, H et a].: Chem Pharm Bull (CPBTAL) 24,632 (1976)

Giannella, M et al.: Chim Ther (CHTPBA) 7, 127 (1972)

oral formulation:

JP 63 150 220 (Dainippon; appl 15.12.1986)

alternative synthesis:

Mohareb, R.M et a].: Z Naturforsch., B: Chem Sci (ZNBSEN) 45, 1067 (1990)

Formulation(s): powder 200 mglg; tabl 100 mg

Trade Narne(s):

J: Excegran (Dainippon;

1990)

Zopiclone

(RP-27267)

ATC: NOSBX; NOSCFO1 Use: anxiolytic, hypnotic RN: 43200-80-2 MF: C,,H,,CIN601 MW: 388.82 EINECS: 256-138-9

LD5,,: 580 mglkg (M, i.p.); 321 mg/kg (M, i.v.); 2174 mglkg (M, p.0.);

280 mglkg (R, i.v.); 827 mglkg (R, p.0.);

400 mglkg (dog, i.v.); 2500 mglkg (dog, p.0.)

CN: 4-methyl-1 -piperazinecarboxylic acid 6-(5-chloro-2-pyridinyl)-6,7-dihydro-7-oxo-5H-py~olo[3,4- blpyrazin-5-yl ester

pyrozine-2,3- 2-amino-5- 3-(5-chloropyrtd-2-yl- 6-(5-chloropyrld-2-yI)-

d~corboxylic chloropyr~d~ne corbarnoyl)pyrilz~ne-2- 5,7-dioxo-6,7-dihydro-

4->1 - 1 -chlorocorbonyl-4-

methylpiperazine

0

Zopiclone

Referencefs):

DOS 2 300 491 (RhBne-Poulenc; appl 5.1.1973; F-prior 7.1.1972,9.9.1972)

US 3 862 149 (RhBne-Poulenc; 21.1.1975; F-prior 7.1.1972,9.9.1972)

Formulation(s): f c tabl 7.5 mg

Trade Name(s):

D: Ximovan (RhBne-Poulenc GB: Zimovane (RhBne-Poulenc J: Amoban (RhBne-Poulenc-

F: Imovane (Specia Groupe I: Imovane (RhBne-Poulenc

RhBne-Poulenc Rorer) Rorer; 1989)

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