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Pharmaceutical Substances Syntheses, Patents, Applications - Part 101 pptx

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autolysis of comminuted tissue parts, heating with ammonium sulfate in alkaline solution, filtration and acidification yield heparin as complex with protein, removal of fat with alcohol

Trang 1

Heparin H 1001 Uzara plus (Uzara)-comb.; GB: Quixalin (Squibb); wfm

Use: anticoagulant, antithrombotic RN: 9005-49-6 MF: [C,,H,,N,O,sS,]x MW: unspecified EINECS: 232-681-7

LD,,,: 500 mglkg (M, i.v.);

1950 mglkg (R, p.0.)

CN: mucopolysaccharide polysulfuric acid ester

sodium salt

RN: 9041-08- 1 MF: unspecified MW: unspecified

LD,: 2800 mgikg (M, i.v.); >5 g k g (M, p.0.);

391821 i d k g (R, i.v.); >779000 i d k g (R, p.0.);

I glkg (dog, i.v.)

calcium salt

RN: 37270-89-6 MF: unspecified

LD,,: A 0 g k g (M, i.v.);

>40 gikg (R, i v.)

magnesium salt

RN: 54479-70-8 MF: unspecified

MW unspecified

MW: unspecified

(molar mass 6000-20000, according to origin)

From animal tissue, especially bovine lung and liver (e g autolysis of comminuted tissue parts, heating with ammonium sulfate in alkaline solution, filtration and acidification yield heparin as complex with protein, removal

of fat with alcohol and treatment with trypsine for the purpose of decomposition of proteins, precipitation with alcohol and various purification methods)

Reference(s):

review:

Hind, H.G.: Manuf Chem (MACSAS) 34,510 (1963)

purification:

US 2 884 358 (Southerm California Gland Co; 28.4.1959; appl 22.4.1957),

US 2 989 438 (Uclaf; 20.6.1961; appl 29.12.1958)

DE 1 195 010 (Ormonoterapia Richter; appl 12.5.1962)

US 3 016 331 (Ormonoterapia Richter; 9.1.1962; I-prior 28.1.1960)

US 4 119 774 (AB Kabi; 10.10.1978; appl 2.3.1977)

GB 1 539 332 (AB Kabi; appl 4.3.1977; S-prior 5.3.1976)

Formulation(s): amp 12500 iu, 20000 iu, 50000 iu, 60000 iu; cream, eye drops and eye ointment 30000 iu,

60000 iu, 150000 iu (as sodium salt or calcium salt); syringe 5000 iu, 7500 iu

Trang 2

Trade Name(s):

D: Calciparin (Sanofi

Winthrop)

Heparin-lnjekt (Immuno)

Heparin-Na (Braun

Melsungen; medac;

Nattermann; ratiopharm)

Heparin Novo (Novo)

Heparin POS (Ursapharm)

Heparin Riker (Riker)

Liquemin (Roche)

Thrombareduct

(Azuchemie)

Thrombophob (Knoll)

Traumalitan (3M M e d ~ c a ;

as sodium salt)

Vetren (Klinge)

numerous generic and

combination preparations

F: Calciparin (Sanofi

Winthrop; as calcium salt)

Dioparine (ThCa; as sodium

salt)

NCoparyl Framycttine

(CIBA Vision

0phthalmics)-comb

numerous generic and

combination preparations

GB: Canusal (CP Pharm.) Clexane (RhGne-Poulenc Rorer)

Fragmin (Pharmacia &

Upjohn) Hepsal (CP Pharm.) Monoparin (CP Pharm.) generic and combination preparations

I: Ateroclar (Mediolanum) Chemyparin (SIT) Clarisco (Schwarz) Disebrin (Allergan) Eparina (Tariff Integrativo;

Bristol-Myers Squibb;

Manetti Roberts; Parke Davis)

Eparinovis (Intes) Essaven Gel (RhGne- Poulenc Rarer)-comb

Flebs Crema (Pierre Fabre Phar.)-comb

Heparin Collirio (Farmigea) Idracemi Eparina (Farmigea)-comb

Lioton (Menarini)

Liquemin (Roche; as sodium salt) Luxazone Eparina (Allergan)-comb

Normoparin (Opocrin) Venotrauma (Also)-comb Viteparin (Teofarma)- comb

numerous generic preparations J: Caprocin (Mitsui; as

calcium salt) Depo-Heparin (Upjohn- , Kodama; as sodium salt) Hepacarin (Eisai) Heparigen (Mukasa-Torii) Heparin Sodium (Tokyo Tanabe)

Novo Heparin (Novo- Kodama)

Panheprin (Nippon Abbott) numerous generic preparations USA: Heparin-Sodium (Wyeth- Ayerst)

Hep-Lock (Elkins-Sinn)

Use: vasodilator RN: 7237-81-2 MF: C2,H3,N,06 MW: 505.57

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

CN: 3-pyr~d~necarboxylic acid 2-hexyl-2-[[(3-pyr1d1nylcarbonyl)oxy]methyl]-1,3-propaned1yl ester

octanol

0

H 0

2-hexyl-2-hydroxy- methyl- 1,3-

proponediol (I)

chloride

Trang 3

Heptabarb H 1003

Reference(s):

U S 3 384 642 (Yoshitomi; 21.5.1968; J-prior 18.11.1964, 12.10.1965)

Formulation(s): tabl 100 mg

Trade Name(s):

I: Megrin (Yoshitomi)

(Heptabarbital; Heptabarbitone; Heptamalum) Use: hypnotic sedative

RN: 509-86-4 MF: Cl3HI8N2O3 MW: 250.30 EINECS: 208-107-6

LD,,: 180 mglkg (M, i.v.); >800 mglkg (M, p.0.);

>S glkg (R, p.0.);

105 mglkg (dog, i.v.)

H$"B~ , N O O C H ~

-+I

cyanaacetate

Reference(s):

FR 870 714 (Geigy; appi 1941 ; Palestine-prior 1940)

DE 756 489 (Geigy; appl 1941 ; Palestine-prior 1940)

Forrnulation(s): tabl 200 mg

Trade Name(s):

D: Medomin (Geigy); wfm F: Medomine (Geigy); wfm GB: Medomin (Gcigy); wfm

Use: cardiotonic, sympathomimetic RN: 372-66-7 MF: C8Hl9NO MW: 145.25 EINECS: 206-758-0

LD,,,: 1250 mgikg (M, i.p.)

CN: 6-amino-2-methyl-2-heptanol

hydmchloride

RN: 543-15-7 MF: C,H,,NO HCI MW: 181.71 EINECS: 208-837-5

LD,,: 900 mglkg (M, i.p.)

Trang 4

1004 H Hetacillin

5-hepten-2-one

~ejizrence(s):

Dceuvre, I.; Pozat, I.: C R Hebd Seances Acad Sci (COREAF) 224,286 (1947)

Formulation(s): amp 250 mg, 500 mg; drg 50 mg; drops 50 mg/ml;tabl 150 mg (as hydrochloride)

Trade Name(s):

D: Normotin (0TW)-comb DCbmmyl (Pierre Fabre numerous combination

F: Amptcyclal (Sargel) Sureptil (SynthClab0)- I: Coreptil (Delalande

Use: antibiotic RN: 3511-16-8 MF: C,,HZ3N3O4S MW: 389.48 EINECS: 222-512-5

azabicyclo[3.2.0]heptane-2-carboxylic acid

monopotassium salt

RN: 5321 -32-4 MF: C,,H,KN,04S MW: 427.57 EINECS: 226-182-3

LD,,,: 650 mglkg (M, i.v.); >15 g k g (M, p.0.);

>1400 m g k g (R, i.v.); > I 0 gikg (R, p.0.);

2200 m g k g (dog, 1.v.); >4 g k g (dog, p.0.)

ONa

(q v )

Reference(s):

US 3 198 804 (Bristol-Myers; 3.8.1965; appl 6.1.1965; prior 25.1.1963)

Formulation(s): amp 250 mg, 500 mg, 1 g; tabl 5 0 mg (as potassium salt)

Trade Name(s):

D: Penplenum (Bristol); wfm Etadipen (Ghimas)-comb J: Natacillin (Banyu)

F: Versapen (Allard); wfm with dicloxacillin; wfm USA: Versapen (Bristol); wfm

I: Dicloeta (Lusopharma)- Versaclox (Bristo1)-comb

comb with dicloxacillin; with dicloxacillin; wfm

Trang 5

Heteronium bromide H 1005

Use: anticholinergic

RN: 7247-57-6 MF: C , *H,,BrN03S MW: 41 2.35

LDs,,: 3576 mgkg (R, p.0.)

CN: 3-[(hydroxyphenyl-2-thienylacety1)oxyl-1 ,l-dimethylpyrrolidinium bromide

NaOCH,, n-C7HI6

I-methyl- phenyl-

3-pyrrolidinol (2-thieny1)-

glycolic

acid

H,C-Br

methyl

bromide

I Heteroniurn bromide

u s 3 138 614 (Eli Lilly; 23.1.1964; prior 18.12.1961, 3.8.1960)

slarting material:

US 2 830 997 (A H Robins; 1958; prior 1956)

Formulation(s): tabl 1 mg

Trade Name(s):

I: Quentar (Ravizza)-comb USA: Hetrum Bromide (Lilly);

Use: topical antiinfective, disinfectant, parasiticide

RN: 70-30-4 MF: C,,H6c160, MW: 406.9 1 EINECS: 200-733-8

LD,,: 67 mgkg (M, p.0.);

7500 @kg (R, i.v.); 56 mglkg (R, p.0.)

Trang 6

1006 H Hexafluronium bromide

2 NaOH

+ (CH,O),

Refirence(s):

US 2 250 480 (B T Bush; 1941; appl 1939)

US 2 435 593 (B 1Bush; 1948; appl 1945)

US 2 8 12 365 (Givaudan Corp.; 1957; prior 1951, 1954)

2,4.5-trichloro- poroform-

Forniulation(s): cream 0.5 g1100 g; emulsion 0.5 gt100 g; lotion 0.5 gt100 g

Hexachlorophene

Trade Narne(s):

D: Aknefug (Wolff) GB: Dermalex (Sanofi Phisohex disinf (Magg~om-

with estrad~ol Ster-Zac D.C (Seton) Vestene (Eurospital); wfm

F: Acnestrol (Po1rier)-comb 1: Etaproctene (Ange1ini)- USA: pHisoHex (Sanofi)

comb.; wfm

f

RN: 3 17-52-2 MF: C,,H,,Br2N2 MW: 662.55 EINECS: 206-265-0

Hexafluronium bromide

US 2 783 237 (Irwin, Neisler & Co.; 1957; prior 1953)

F r t i o ( ) : amp 20 mgln~l

1

Trade Name(s):

J : Mylaxen (Nippon Shoji); USA: Mylaxen (Mallinckrodt); Mylaxen (Wallace); wfm

Trang 7

Hexamethonium chloride H 1007

Use: ganglionic blocker, antihypertensive RN: 60-25-3 MF: CI2H3,Cl2N2 MW: 273.29 EINECS: 200-465-1

LD,,,: 26.7 mglkg (M, i.v.);

35 mgkg (dog, i.v.)

CN: N, N, N,N,N,N-hexamethyl- 1,6-hexanediaminium dichloride

CH3

Reference(s):

DE 900 097 (May & Baker; appl 195 1 ; GB-prior 1950)

H3C\+

Formulation(s): oral: 0.5 gld

Trade Name(s):

D: Raucombin forte (Voigt); Gastrometonio (Fabo; as

1: Gastrometonio (Fabo); J: Methobromin

Hexcarbacholine bromide

(Carbolonium bromide)

ATC: M03 Use: muscle relaxant

RN: 306-41-2 MF: C,,H,,,Br,N,O, MW: 536.35

H

thionyl

methylene- carbonate

diamine

Trang 8

1008 H Hexestrol ":

1 potassium bromide

2 trimelhylamine

H

1 Hexcorbacholine bromide 1

Reference(s):

DE 1 021 842 (Osterr Stickstoffwerke; appl 1954; A-prior 1953)

Formulation(s): amp 2 mglml

Trade Narne(s):

D: lmbretil (Hormon-

Chemie); wfm

Use: estrogen, antineoplastic (hormonal) RN: 84-16-2 MF: C1XH2202 MW: 270.37 EINECS: 201-518-1

LDs": 1 g/kg (M, p.0.);

>2 glkg (R, p.0.)

@ W 3 r , ether, toluene, CoCI2

b

1 -bromo-1-(4-meth-

oxypheny1)propone (I)

(cf diethylstilbestrol

synthesis)

HI

11 -*

hydrogen

iodide

1 metals (Na Mg Ai, or Fe)

2 HI

1

1 (sodium, magnesium, aluminum, or iron)

2 hydrogen iodide

Trang 9

Hexetidine H 1009

Reference(s):

a Kharasch, M.S.; Kleimann, M.: J Am Chem Soc (JACSAT) 65,491 (1943)

b Dodds, E.C et a].: Proc R Soc London, Ser B (PRLBA4) 218,253 (1940)

Bernstein, S.; Wallis, E.S.: J Am Chem Soc (JACSAT) 62, 2871 (1940)

Buu-Hoi', N.G.; Hoan, N.G.: J Org Chem (JOCEAH) 14, 1023 (1949)

US 2 357 985 (Research Corp; 1944; appl 1940)

GB 523 320 (Boots; appl 1938)

FR 855 879 (Lab Franc; de ChimiothCrapie; appl 1939)

starting material:

Bemstein, S.; Wallis, E.S.: J Am Chem Soc (JACSAT) 62,2871 (1940)

alternative syntheses:

Dockcn, A.M.; Spielman, M.A.: J Am Chem Soc (JACSAT) 62,2163 (1940)

US 2 392 852 (Lilly; 1946; prior 1941)

US 2 402 054 (Lilly; 1946; prior 1941)

US 2421 401 (Hoffmann-La Roche; 1947; S-prior 1943)

review:

Solmssen, U.V.: Chem Rev (Washington, D C.) (CHREAY) 36,481 (1945)

Fonulation(s): pessaries 10 mg

Trade Name(s):

D: Malun (Temm1er)-comb.;

F: Cycloestrol (Bruneau); J:

wfm

Micro-cristaux Cycloestrol USA:

(Bruneau); wfm

Synthrogene (Gerda); wfm Hexestrol and Phenorbital Synthovo (Boots); wfm (Jenkins)-comb.; wfm Robal (Chugai; as Hexestrol WlButabarb

Estra-Plex (Rowell); wfm Vagi-Plex (Rowell)-comb.;

wfrn

Use: antiseptic antifungal RN: 141-94-6 MF: C2,H4,N3 MW: 339.61 EINECS: 205-513-5

Reference(s):

US 2 415 047 (Commercial Solvents; 1947; appl 1945)

US 3 054 797 (Commercial Solvents; 18.9.1962; prior 1 1.10.1961),

Senkus, M.: J Am Chem Soc (JACSAT) 68,161 1 (1946)

Trang 10

1010 H Hexobarbital

pur$cation:

DE 2 01 1 078 (Godecke; appl 9.3.1970)

DAS 2 355 917 (Meditest; appl 8.1 1.1973)

DOS 2 709 929 (Dolorgiet; appl 8.3.1977)

DOS 2 310 337 (Wiilfing; appl 1.3.1973)

DAS 2 323 150 (Wiilfing; appl 8.5.1973)

salts with aromatic acids:

GB 1 538 603 (Doll; appl 5.1 1.1976; D-prior 6.11.1975, 3.6.1976, 16.6.1976)

US 4 141 968 (Doll; 27.2.1979; D-prior 16.6.1976)

US 4 142 050 (Doll; 27.2.1979; D-prior 6.1 1.1975,3.6.1976)

nicotinate:

DOS 2 310 338 (Wiilfing; appl 1.3.1973)

Fortnulation(s): sol 100 mg1100 ml, 200 mg1100 ml; spray 0.1 d l 0 0 g; vaginal tabl 10 mg

Trade Namc(s):

D: Anginasin Spray

(0pfermann)-comb

De-menthasin (Scheurich)-

comb

Doreperol (Rentschler) F:

Givalex (Norgine)-comb

Hexetidin Gurgellosung

(ratiopharm)

Hexoral (Warner-Lambert) Nifluril (UPSA) Hcxoral Spray (Warner- GB: Oraldene (Wamer-

Collu-Hextril (Warner- USA: Sterisil (Warner Chilcott);

Givalex (Norgine)-comb

Hextril (Warner-Lambert)

Use: hypnotic, sedative RN: 56-29- 1 MF: C,,Hl6N,O3 MW: 236.27 EINECS: 200-264-9

LD,,,: 133 mglkg (M, i.v.); 468 mglkg (M, p.0.)

CN: 5-(1 -cyclohexen- 1 -yl)- 1,s-dimethyl-2,4,6(1 H,3H,SH)-pyrimidinetrione

sodium salt

RN: 50-09-9 MF: C12H1,N,Na0, MW: 258.25 EINECS: 200-009-1

LD,,,: 165 mglkg (M, i.v.); 1325 mglkg (M, p.0.);

1 gikg (R, p.0.)

O+ /O'CH~

H ~ c ~ / ~ + ~ , NoOCH3

hexonone cyono- 1 -cyclohexenyl-

acetate cyonoocetate

H + H2NKN\CN

methyl 2-cyano- dicyono-

2-(1 -cyclohexenyl)- diomide

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