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Pharmaceutical Substances Syntheses, Patents, Applications - Part 5 pps

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formulations: injection form: EP 136 463 Bioresearch; appl.. gastric juice resistant form: EP 136 464 Bioresearch; appl... 20 ml with 300 mg meglumine salVml triiodobenzaic acid cf.

Trang 1

Adiphenine A 41

4-toluenesulfonate sulfates:

US 3 954 726 (Bioresearch; 4.5.1976; I-prior 27.6.1973; 24.5.1974)

other sulfonates:

DOS 2530 898 (Bioresearch; appl 10.7.1975; I-prior 12.7.1974)

US 4057 686 (Bioresearch; 8.1 1.1977; I-prior 12.7.1974)

US 4 465 672 (Bioresearch; 14.8.1984; I-prior 24.8.1981)

EP 72 980 (Bioresearch; appl 12.8.1982; I-prior 24.8.1981)

EP 162 323 (Bioresearch; appl 25.4.1985; I-prior 16.5.1984)

EP 162 324 (Bioresearch; appl 25.4.1985; I-prior 16.5.1984)

other salts:

EP 73 376 (Bioresearch; appl 12.8.1982; I-prior 24.8.1981)

EP 74 555 (Bioresearch; appl 30.8.1982; I-prior 11.9.1981)

EP 108 817 (Kanegafuchi; appl 6.11.1982)

EP 141 462 (Tecofar; appl 19.10.1984; I-prior 26.10.1983)

formulations:

injection form:

EP 136 463 (Bioresearch; appl 1.8.1984; I-prior 24.8.1983)

gastric juice resistant form:

EP 136 464 (Bioresearch; appl 1.8.1984; I-prior 24.8.1983)

Formulation(s): amp 384 mg; tabl 384 mg (as bisulfate)

Trade Name(s):

I: Donamet (Knoll) Transmetil (Bioresearch)

Use: antispasmodic, anticholinergic RN: 64-95-9 MF: C,oH25N02 MW: 31 1.43 EINECS: 200-599-0

LD,,: 182 rnglkg (M, i.p.); 21.5 mglkg (M, i.v.); 600 mglkg (M, p.0.); 400 mglkg (M, s.c.);

27 mgkg (R, i.v.);

35 mgkg (dog, i.v.);

30 mgfkg (rabbit, i.v.)

CN: a-phenylbenzeneacetic acid 2-(diethy1amino)ethylester

hydrochIoride

RN: 50-42-0 MF: C2,H2,N02 HCI MW: 347.89 EINECS: 200-036-9

LD,,: 185 mglkg (M, i.p.); 500 mglkg (M, p.0.); 650 mglkg (M, LC.);

250 mglkg (R, i.p.); 17.3 mgkg (R, i.v.)

<CH, HO&N-CH3 _*

ethanol

Reference(s):

DE 626 539 (Ciba; 1934)

drg 20 mg, 25 mg; suppos 40 mg, 50 mg

Trang 2

42 A Adipiodone

Trade Name(s):

F: Spasmo-Cibalgine (Ciba)- I: Nisidina (De Angel+ USA: Trasentine (Ciba); wfm

Adipiodone

(Iodipamide)

ATC: V08AC04 Use: X-ray contrast medium

RN: 606-17-7 MF: C2,H,,IhN20, MW: 11 39.76 EINECS: 210-105-5

LD,,: 2440 m g k g (M, i.v.)

CN: 3,3'-[(I ,6-dioxo-1,6-hexanediyl)diimino]bis[2,4,6-triiodoben~0i~ acid]

disodium salt

RN: 2618-26-0 MF: C,,H,,I,N,Na,O, MW 1183.73 EINECS: 220-049-3

LD,,: 3400 m g k g (R, i.v.)

meglumine salt (1:2)

RN: 3521-84-4 MF: C2,H,,IhN20~ 2C7H,,N05 MW: 1530.19 EINECS: 222-534-5

LD,,: 3195 m g k g (M, i.v.);

5000 m g k g (R, i.v.); 1921 m g k g (R, parented);

1446 m g k g (rabbit, parenteral);

1200 m g k g (dog, i.v.)

Reference(s):

US 2 776 241 (Schering AG; 1957; D-prior 1952)

DE 936 928 (Schering AG; appl 1952)

DE 962 698 (Schering AG; appl 1952)

DE 962 699 (Schering AG; appl 1953)

DE 1 006 428 (Schering AG; appl 1955)

3-amino-2.4,6- odipoyl chloride

starting material:

Kretzer, H.: Ber Dtsch Chem Ges (BDCGAS) 30, 1944 (1897)

Adipiadone

Formulation(s): amp 20 ml with 300 mg meglumine salVml

triiodobenzaic

acid

(cf ocetrizaic

acid synthesis)

Trade Name(s):

D: Biligrafin (Schering); wfm Endografin (Schering Endografin (Schering- Endografin (Schering); Chemicals); wfm Nichidoku; as meglumine

F: Transbilix (Guerbet; as Endocistobil (Bracco); wfm USA: Cholografin (Squibb); wfm meglumine salt) J: Biligrafin (Schering- Cholografin Meglumin

Chemicals); wfrn

Trang 3

Adrafinil A 43

Adrafinil

(CRL-40028)

ATC: N06BX17 Use: a-adrenergic agonist (for symptomatic treatment of vigilance and depresswe manifestations), antidepressant

RN: 63547-13-7 MF: C,,H,,NO,S MW: 289.36 EINECS: 264-303-1

LD,,,: >2048 mglkg (M, i.p.); 1950 m g k g (M, p.0.)

CN: 2-[(diphenylmethyl)sulfinyl]-N-hydroxyacetamide

thiourea chlaroacetic acid S-COOH

benzhydrol diphenyl-

rnethanethiol

(benzhydry1thia)-

acetic acid (I)

1 (H,CO),SO,, NaHCOJ

2 N H 2 0 H , NaOH

hydrogen $-COOH 1 dirnethyl sulfate

peroxide 2 2 hydroxylarnine

(benzhydrylsulfi- Adrafinil nyl)ocetic acid

1 CZH,OH, H2S0,

2 N H 2 0 H , KOH

I H z 0 2

2 hydroxylornine

hydrogen

0

peroxide

Reference(s):

DOS 2 642 51 1 (Lab Lafon; appl 22.9.1976; GB-prior 2.10.1975)

US 4 066 686 (Lab Lafon; 3.1.1978; GB-prior 2.10.1975)

US 4 098 824 (Lab Lafon; 4.7.1978; GB-prior 2.10.1975)

Trade Name(s):

F: Olmifon (Lafon; 1985)

Use: sympathomimetic, vasoconstrictor, hernostyptic

RN: 99-45-6 MF: C,H,,NO, MW: 181.19 EINECS: 202-756-9

LD,,: 275 mgfkg (M, i.v.)

CN: 1-(3,4-dihydroxypheny1)-2-(methy1amino)ethanone

hydrochloride

RN: 62-13-5 MF: C,H,,NO, HCI MW: 217.65 EINECS: 200-525-7

LD,,,: 902 mglkg (M, i.p.)

Trang 4

44 A Afloqualone

chloroocetic cotechol

acid

2-chloro-3'.4'- dihydroxy- ocetophenone (I)

I Adrenalone

H3C-NH,

I b

rnethylomine

Reference (s):

DRP 152 8 14 (Hoechst; 1903)

OH

Trade Name(s):

D: Stryphnasal (Sertiimer) F: Adrtnalone Tktracaine HCrnorrodine (Rocher)-

Guillon (Pharmascience)- comb.; wfrn comb.; wfm

Use: muscle relaxant RN: 56287-74-2 MF: C1,Hl4FN3O MW: 283.31

LDso: 397 mglkg (M, p.0.);

249 mglkg (R, p.0.)

hydrochloride

RN: 56287-75-3 MF: C,,H,,FN,O xHC1 MW: unspecified

SOCI,

5-nitroonthronilic

H 3 C N-(2-amino-5-nitro-

fluoroocetyl

Trang 5

Ajmaline A 45

-

Reference(s):

DOS 2 449 11 3 (Tanabe; appl 15.10.1974; J-prior 15.10.1973)

US 3 966 73 1 (Tanabe; 29.6.1976; J-prior 15.10.1973)

Tani, J et al.: J Med Chem (JMCMAR) 22, 95 (1979)

Formulation(s): tabl 20 mg

Trade Name(s):

J: Aflospan (Kyowa) Arofuto (Tanabe; 1983)

Ajmaline

(Rauwolfine)

ATC: COlBAO5 Use:- antiarrhythmic RN: 4360-12-7 MF: C,oH26N202 MW: 326.44 EINECS: 224-439-4

LD,,: 75 m g k g (M, i.p.); 21 m g k g (M, i.v.); 255 mgkg (M, p.0.); 180 m g k g (M, s.c.);

94 m g k g (R, i.p.); 26 mglkg (R, i.v.); 360 m g k g (R, p.0.); 216 mglkg (R, s.c.)

CN: (l7RJl a)-ajmalan-l7,21-diol

monohydrochloride

RN: 4410-48-4 MF: C20H26N202 HC1 MW: 362.90 EINECS: 224-562-3

LDso: 105 mg/kg (M, i.p.); 26 m g k g (M, i.v.); 205 m g k g (M, p.0.);

86 m g k g (R, i.p.); 19.3 m g k g (R, i.v.); 290 m g k g (R, p.0.);

135 mg/kg (g p., p.0.)

I Ajrnoline

By extraction from the pulverized roots of Rauwolfia serpentina (L.) Beuth

Reference(s):

Siddiqui, S.; Siddiqui, R.H.: J Indian Chem Soc (JICSAH) 8, 667 (1931); 9, 539 (1932); 12, 37 (1935)

Formulation(s): amp 2 mg12 ml, 50 mg/2 ml, 10 mgIlO ml, 50 mg/lO ml

Trade Name(s):

D: Gilurytmal (Solvay F: Cardiorythmine (Servier); Ritmosedina (Inverni della

Tachmalin (ASTA Medica Dipaxan (1nnothCra)- J: Gilurytmal (Giulini-Tokyo

I: Aritmina (UCM)

Trang 6

4 6 A Alacepril

Alacepril

(DU-1219)

ATC: C09A Use: antihypertensive (ACE inhibitor), metabolizes partly to captopril RN: 74258-86-9 MF: C20H2hN20SS MW: 406.50

LD,,: >5 glkg (M, p.0.);

>5 glkg (R, p.0.)

CN: (S)-N-[l-[3-(acetylthio)-2-methyl-l-oxopropyl]-~-prolyl]-~-phenylalanine

1 THF N-methylmarpholine ~ O ~ , -15 C O C I

-

b 1

1 phenyl chloroformote

CH3 2 L-phenylalonine tert-butyl ester

1 -[(S)-3-ocetylthio- hydrochloride

2-methylpraponoyl]-

L-proline

(cf captopril synthesis)

Referencefs):

US 4 248 883 (Dainippon Pharmac Co.; 3.2.1981; J-prior 6.7.1978)

EP 7 477 (Dainippon Pharmac Co.; appl 3.7.1979; J-prior 6.7.1978)

pharrnmology:

Takeyama, K et al.: Arzneim.-Forsch (ARZNAD) 35, 15U2 (1985)

metabolistn:

Matsumoto, K et al.: Arzneim.-Forsch (ARZNAD) 36,40 (1986)

Formulation(s): tabl 12.5 mg, 25 mg

Trade Name(s):

J: Cetapril (Dainippon; 1988)

Use: non-essential proteinogenic amino acid (part of infusion solutions) RN: 56-41-7 MF: C3H7N02 MW: 89.09 EINECS: 200-273-8

CN: L-alanine

Trang 7

Alatrofloxacin mesilate A 47

enzyrn rocernote resolution

1 with ominoocylose

H3C COOH

enzym rocernote resolution

NaOH with orninoocylose

L-Alonine

enzyrn decorboxylotion with L-osportote 8-decorboxylose, '

YH2 e.g in irnrnobil Pseudomonos docunhoe (IAM 1152)

HOOC+

COOH

L-osporoginic

acid

Reference(s):

review:

Ullmann's Encyclopedia of Industrial Chemistry, 5th Ed., Vol A2,69

Kaneko, T.; Izumi, Y.; Chibata, I.; Itoh, T.: Synthetic Production and Utilization of Amino Acids, Kodansha Ltd and John Wiley & Sons, Tokyo, New York, p 62 (1974)

c US 3 898 128 (Tanabe; 5.8.1975; J-prior 20.11.1972)

Yamamoto, K et a].: Biotechnol Bioeng (BIBIAU) 22, 2045 (1980)

Formulation(s): tabl 400 mg

Trade Name(s):

F: Theraplix (Abufene)

Alatrofloxacin mesilate

(CP 116517; CP 116517-27)

ATC: JOlMA Use: antibacterial, prodrug of trovafloxacin

RN: 146961-77-5 MF: C2,H2,F3N605 CH403S MW: 654.62

naphthyridin-2-yl]-3-azabicyclo[3.1 O]hex-6-yl]-L-alaninamide monomethanesulfonate

base

RN: 146961-76-4 MF: C2,H2,F3N,0, MW: 558.52

Trang 8

48 A Alclofenac

-

H,C-S03H

acetane/H20

11

rnethanesulfonic

acid

dihydroquinoline

(EEDP)

F

Alatrofloxacin rnesilate

US 5 164 402 (Pfizer; 17.1 1.1992; appl 4.2.1991; WO-prior 16.8.1989)

WO 9 700 268 (Pfizer; appl 27.3.1996; USA-prior 15.6.1995)

Formulation(s): vials 200 mgl40 ml, 300 mg160 ml(5 mg/ml) (as mesilate)

Trade Narne(s):

D: TROVAN (Pfizer); wfm GB: Turvel (Pfizer); wfm USA: Trovan (Pfizer); wfm F: Turvel (Pfizer); wfm I: Turvel (Pfizer); wfm

Use: analgesic, antipyretic, anti- inflammatory

RN: 22131-79-9 MF: CIIH,,C103 MW: 226.66 EINECS: 244-7954

LD,,: 508 mg/kg (M, i.p.); 1100mg/kg (M, p.0.);

465 mglkg (R, i.p.); 1050 mg/kg (R, po.)

CN: 3-chloro-4-(2-propeny1oxy)benzeneacetic acid

sodium salt

RN: 24049-1 8-1 MF: C,,H,,ClNaO, MW: 248.64

LD,,: 530 m g k g (R, i.p.); 1050 mg/kg (R, p.0.)

Trang 9

Alclometasone dipropionate A 49

ollyl bromide (1) 2-chloraphenol 2-chlorophenyl ally1 ether (n)

HCI, A s 2 0 3 NoCN DMSO

I1 + HCHO -

sodium cyonide ' 111

CI

formolde- 4-ollyloxy-3-chloro-

CI

4-allyloxy-3-chloro-

benzyl cyanide (nI)

3-chloro-4-hydroxy-

benzoldehyde

benzyltrimethyl- ammonium hydroxide

formoldehyde

dimethyl mercoptol

S-oxide

Alclofenoc

4-allyloxy-3-chloro- benzoldehyde (IV)

1 -(2-methylsulfinyl-2-methyl-

thioviny1)-4-ollyloxy-3-

chlorobenzene

Reference(s):

a BE 704 368 (Madan; appl 27.9.1967)

BE 718 930 (Madan; appl 1.8.1968; prior 27.9.1967)

GB 1 174 535 (Madan; appl 28.8.1968; B-prior 27.9.1967, 1.8.1968)

b GB 1 504 828 (Sagami; appl 26.1 1.1976; J-prior 1.12.1975)

lysine salt:

DOS 2 71 1 964 (Biochcfarm; appl 18.3.1977)

Formulation(s): amp 833 mg; tabl 1 g, 500 mg

Trade Nanze(s):

D: Neoston (Beiersdorf); wfm I: Rentenac (Tosi); wfm J: Allopydin (Chugai)

GB: Prinalgin (Berk); wfm Zumaril (Sidus); wfm Epinal (Mitsubishi Yuka)

Use: topical steroidal anti-inflammatory (glucocorticoid)

RN: 66734- 13-2 MF: C2,H&1O7 MW 521 .O5 EINECS: 266-464-3

LD,,: 2506 mgkg (M, s.c.);

3593 mgkg (R, s.c.)

CN: (7a, 1 lb,l6a)-7-chloro-l l -hydroxy-16-methyl-l7,21-bis(l-oxopropoxy)pregna-l,4-diene-3,2O-dione

Trang 10

50 A Alclometasone dipropionate

16a-methylprednisolone

21 -ocetote

(intermediate of

dexarnethasone

synthesis)

, HCI, dioxane,

0

room temp 24 h

b

2.3-dichloro-5.6-dicyano- benzoquinone (0012)

16a-methyl-21 -acetoxy-

1 lfl.17n-dihydroxypregna- 1,4,6-triene-3.20-diane (I)

triethyl orthopropionate

H ~ C / ~ ~ V C H , , pyridine

0 0

I V

propionic anhydride (V)

HCI, dioxane

VI -+

Alclometasone dipropiontlte

hue, H.-J.; Green, M.J.: J Med Chem (JMCMAR) 23,430 (1980)

US 4 124 707 (Schering Corp.; 7.1 1.1978; prior 12.12.1976,7.11.1977)

US 4 076 708 (Schering Curp.; 28.2.1978; prior 22.12.1976)

DOS 2 756 550 (Scherico; appl 19.12.1977; USA-prior 22.12.1976)

Formulation(s): cream and ointment 0.5 mgll g

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