[go: up one dir, main page]

US3652567A - Quinazolinone derivative and process for the production thereof - Google Patents

Quinazolinone derivative and process for the production thereof Download PDF

Info

Publication number
US3652567A
US3652567A US866719A US3652567DA US3652567A US 3652567 A US3652567 A US 3652567A US 866719 A US866719 A US 866719A US 3652567D A US3652567D A US 3652567DA US 3652567 A US3652567 A US 3652567A
Authority
US
United States
Prior art keywords
methyl
quinazoline
hydroxypropyl
phenylpiperazine
compound
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US866719A
Inventor
Karl-Heinz Boltze
Dietrich Lorenz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Troponwerke Dinklage and Co
Original Assignee
Troponwerke Dinklage and Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Troponwerke Dinklage and Co filed Critical Troponwerke Dinklage and Co
Application granted granted Critical
Publication of US3652567A publication Critical patent/US3652567A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D403/00Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00
    • C07D403/02Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00 containing two hetero rings
    • C07D403/06Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, not provided for by group C07D401/00 containing two hetero rings linked by a carbon chain containing only aliphatic carbon atoms
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/33Heterocyclic compounds
    • A61K31/395Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
    • A61K31/495Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with two or more nitrogen atoms as the only ring heteroatoms, e.g. piperazine or tetrazines
    • A61K31/505Pyrimidines; Hydrogenated pyrimidines, e.g. trimethoprim
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00Details of transformers or inductances, in general

Definitions

  • This invention relates to a new quinazolinone derivative and to a process for the production thereof.
  • the invention provides as a new chemical compound 2-methy1-3- ⁇ 3-[4-phenylpiperazinyl-(1)] 2 hydroxypropyl ⁇ -quinazoline-4-one (hereinafter referred to as I) having the following formula:
  • the LD values with the mouse are very high, being mg./kg. intravenously and 710 mg./kg. per os; 500 mg./ kg. per os are tolerated without reaction by the rabbit. This shows a very low toxicity of the compound I.
  • the compound according to the invention may be prepared by the condensation of l-phenylpiperazine with 2- methyl-3-[3-bromo-2-hydroxypropyl] quinazoline-4-one or by the addition to it of 2-methyl-3- [2,3-epoxypropyl1- quinazoline-4-one or by condensing 2-methylquinazoline- 4-one with epichlorhydrin and then adding to it l-phenylpiperazine preferably without isolation of the intermediate.
  • the invention therefore also provides a process for the preparation of the 2-methyl-3- ⁇ 3 [4 phenylpiperazinyl- (1) ]-2-hydroxypropyl ⁇ -quinazo1ine-4-one in which (a) l-phenylpiperazine is condensed with 2-methyl-3- [3-bromo-2-hydroxypropyl]-quinazoline-4-one or (b) 2 methyl-3-[2,3-epoxypropyl]-quinazoline-4-one is reacted with l-phenylpiperazine; or
  • the reactions can be carried out in the absence of solvents at temperatures above C. and also in the presence of organic solvents, such as ethyl alcohol, at room temperature or higher temperature.
  • the compound according to the invention may be formulated with a pharmaceutical carrier to provide formulations adapted for the particular route of administration in particular the oral route, for example in the form of a syrup, elixir or the like or as a tablet or capsule.
  • EXAMPLE 2 10.8 g. of 2-methyl-3-(2,3-epoxypropyl)-quinazoline-4- one and 8.1 g. of l-phenylpiperazine are boiled for 4 hours in 70 ml. of absolute ethanol and the solution is kept for several hours at room temperature and then in the cold. The substance which precipitates is filtered 01?, the contents of the filter are washed-with ether and then crystallised from ethanol. 14.2 g. of 2-methyl-3- ⁇ 3-[4- phenylpiperazinyl 1 ]-2-hydroxypropyl ⁇ -quinazoline-4- one are formed, corresponding to 75% of the theoretical.
  • EXAMPLE 3 29.2 g. of 2-methylquinazoline-4-one and 70 m1. 82.5 g.) of epichlorhydrin are dissolved in methanol and then an equimolar quantity of sodium methylate in methanol is added. After standing for 12 hours at room temperature, the viscous mass which forms (39.6 g.) is filtered off, removed from the filter and maintained with 44.5 g. of l-phenylpiperazine for 30 minutes in an oil bath at 110 C. The mass (84 g. crude yield) is then worked up as previously described.
  • wa 2-methyl-3- ⁇ 3-[4-phenylpiperaziny1-(1) ]-2-hydroxypropyl ⁇ quinazolin-4-one.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Medicinal Chemistry (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Plural Heterocyclic Compounds (AREA)

Abstract

A QUINAZOLINONE COMPOUND OF THE FORMULA:

2-(CH3-),3-((4-PHENYL-PIPERAZINO)-CH2-CH(-OH)-CH2-),4-(O=)

-QUINAZOLINE

2-METHYL-3-(3-(4-PHENYLPIPERAZINYL-(1)-2-HYDROXYPROPYL)-QUINAZOLINE-4-ONE. THIS COMPOUND HAS ANTITUSSIVE AND ANALGESIC ACTIVITY.

Description

US. Cl. 260---256.4 Q 1 Claim ABSTRACT OF THE DISCLOSURE A quinazolinone compound of the formula:
N-oH,( H-CHt-N 2-methyl-3-{3-[4-phenylpiperazinyl-(1)] 2 hydroxypropyl}-quinazoline-4-one. This compound 'has antitussive and analgesic activity.
on N a This invention relates to a new quinazolinone derivative and to a process for the production thereof.
The invention provides as a new chemical compound 2-methy1-3-{3-[4-phenylpiperazinyl-(1)] 2 hydroxypropyl}-quinazoline-4-one (hereinafter referred to as I) having the following formula:
This compound is effective as an analgesic and antitussive, as more fully described below.
Quinazolinone derivatives are already known and common as drugs for use in human medicine.
As examples of such derivatives there may be mentioned 2-methyl-3-o-tolylquinazoline 4- one, which has anti-convulsive, sedative and hypnotic activity and 2- methyl-3-o-ethylphenylquinazoline -4 one, which has a hypnotic action. In addition certain other quinazolinone derivatives are reputed to be active against malaria.
It has now been found that the aforementioned pharmacological efiects are completely overshadowed in favour of an antitussive and analgesic quality, if the substituted phenyl ring on the quinazolinone skeleton in the 3-position is replaced by a 3-[4-phenylpiperazinyl-(1)]-2- hydroxypropyl group. For example, in the hotplate test on the mouse, the ED (i.e. the dose with which 50% of the animals are protected from pain), amounts to 25 mg./kg. with oral administration, which corresponds in this test approximately to the analgesic effect which results from codeine. In the benzoquinone test (chemical irritation on the peritoneum of the mouse), an ED' of 97 mg./ kg. on oral administration was found, corresponding approximately to the effective strength of the known 1-ethyl-4-methylamino-2,2-diphenylpentyl acetate (dextropropoxyphene). After doses of 25-250 mg./kg. per 0s, and using electrical irritation of the tooth pulp of the rabbit as the test method, the' irritation threshold of the pain was increased by 60-500% with long-lasting effect. In this test, I is even more strongly active than morphine or codeine.
United States Pate 0159c 3,652,567 Patented Mar. 28, 1972 The antitussive eflicacy of the compound was tested on the guinea pig and thecat. With the former, using a sulphuric acid spray as cough irritant, and ED of mg./ kg. was produced with subcutaneous administration, this once again corresponding approximately to the effectiveness of codeine. With the cat (electric stimulation of the laryngicus cranialis nerve) the effectiveness of codeine was reached, with an ED of -l.7 mg./k-g. (intravenous) and 10-20 mg./kg. (enteral). By contrast with the opium alkaloids, when I is used in doses of 5 mg./kg-. intravenously on the unnarcotised rabbit, the respiration (breath intake/breathing phase) is not impaired but it is even improved.
Since sedative, anticonvulsive and hypnotic active components extending into the sub-toxic dose range were not to be found in the appropriate tests, the analgesic and antitussive action cannot be caused by a general central sedation.
The LD values with the mouse are very high, being mg./kg. intravenously and 710 mg./kg. per os; 500 mg./ kg. per os are tolerated without reaction by the rabbit. This shows a very low toxicity of the compound I.
The compound according to the invention may be prepared by the condensation of l-phenylpiperazine with 2- methyl-3-[3-bromo-2-hydroxypropyl] quinazoline-4-one or by the addition to it of 2-methyl-3- [2,3-epoxypropyl1- quinazoline-4-one or by condensing 2-methylquinazoline- 4-one with epichlorhydrin and then adding to it l-phenylpiperazine preferably without isolation of the intermediate.
The invention therefore also provides a process for the preparation of the 2-methyl-3-{3 [4 phenylpiperazinyl- (1) ]-2-hydroxypropyl}-quinazo1ine-4-one in which (a) l-phenylpiperazine is condensed with 2-methyl-3- [3-bromo-2-hydroxypropyl]-quinazoline-4-one or (b) 2 methyl-3-[2,3-epoxypropyl]-quinazoline-4-one is reacted with l-phenylpiperazine; or
(c) 2-methylquinazoline-4-one is first condensed with epichlorhydrin and the product reacted with 1-phenylpiperazine if desired without intermediate isolation.
The reactions can be carried out in the absence of solvents at temperatures above C. and also in the presence of organic solvents, such as ethyl alcohol, at room temperature or higher temperature.
For administration, the compound according to the invention may be formulated with a pharmaceutical carrier to provide formulations adapted for the particular route of administration in particular the oral route, for example in the form of a syrup, elixir or the like or as a tablet or capsule.
The following examples illustrate the invention:
EXAMPLE 1 2.5 g. of 2-methyl-3-(3-bromo-2-hydroxypropyl)-quinazoline-4-one and 2.7 g. of l-phenylpiperazine are maintained for 5 minutes in an oil bath at The melt which is obtained is cooled and chloroform is added to it. The precipitate which is formed (l-phenylpiperazine dihydrobromide) is filtered off, the filtrate is evaporated and the residue crystallised from 96% ethanol. The 2- methy1-3-{3-[4-phenylpiperazinyl-( 1 ]-2-hydroxypropyl}- quinazoline-4-one which is formed melts at 145-144 C.; the yield is 2. 6 g., corresponding to 82% of the theoretical.
For C H N O .--Calculated (percent): C, 69.81; H, 6.93; N, 14.80. Found (percent): C, 70.25; H, 6.66; N, 14.60.
EXAMPLE 2 10.8 g. of 2-methyl-3-(2,3-epoxypropyl)-quinazoline-4- one and 8.1 g. of l-phenylpiperazine are boiled for 4 hours in 70 ml. of absolute ethanol and the solution is kept for several hours at room temperature and then in the cold. The substance which precipitates is filtered 01?, the contents of the filter are washed-with ether and then crystallised from ethanol. 14.2 g. of 2-methyl-3-{3-[4- phenylpiperazinyl 1 ]-2-hydroxypropyl}-quinazoline-4- one are formed, corresponding to 75% of the theoretical.
EXAMPLE 3 29.2 g. of 2-methylquinazoline-4-one and 70 m1. 82.5 g.) of epichlorhydrin are dissolved in methanol and then an equimolar quantity of sodium methylate in methanol is added. After standing for 12 hours at room temperature, the viscous mass which forms (39.6 g.) is filtered off, removed from the filter and maintained with 44.5 g. of l-phenylpiperazine for 30 minutes in an oil bath at 110 C. The mass (84 g. crude yield) is then worked up as previously described.
What is claimed is: wa 1. 2-methyl-3-{3-[4-phenylpiperaziny1-(1) ]-2-hydroxypropyl}quinazolin-4-one.
References Cited 7 UNITED STATES PATENTS 1/1966 Hayao 260-2564 OTHER REFERENCES Morrison et al.: Organic Chemistry1959, Allyn & Bacon, pp. 367, 423.
ALEX MAZEL, Primary Examiner R. V. RUSH, Assistant Examiner US. Cl. X.R.
US866719A 1968-10-16 1969-10-15 Quinazolinone derivative and process for the production thereof Expired - Lifetime US3652567A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19681803210 DE1803210A1 (en) 1968-10-16 1968-10-16 2-Methyl-3- (3- [4-phenylpiperazinyl- (1)] -2-hydroxypropyl) -quinazolinone- (4) and process for its preparation

Publications (1)

Publication Number Publication Date
US3652567A true US3652567A (en) 1972-03-28

Family

ID=5710568

Family Applications (1)

Application Number Title Priority Date Filing Date
US866719A Expired - Lifetime US3652567A (en) 1968-10-16 1969-10-15 Quinazolinone derivative and process for the production thereof

Country Status (7)

Country Link
US (1) US3652567A (en)
CH (1) CH531524A (en)
DE (1) DE1803210A1 (en)
FI (1) FI52725C (en)
FR (1) FR2020814B1 (en)
GB (1) GB1245316A (en)
SE (1) SE378422B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3879393A (en) * 1973-06-18 1975-04-22 Miles Lab Derivatives of 1,3-disubstituted 2,4(1h,3h)-quinazolinediones
DE4203050A1 (en) * 1992-02-04 1992-12-10 Heiko Delecate Combined low voltage solar with compressed air engine - can be operated with solar power or pneumatic motor or as hybrid combination of both
WO2005123694A3 (en) * 2004-06-17 2006-04-13 Novartis Ag Quinazolinone compounds for the treatment of cough
US8552015B2 (en) 2002-02-06 2013-10-08 Novartis Ag Quinazolinone derivatives and their use as CB agonists

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1936588A1 (en) * 1969-07-18 1971-02-18 Troponwerke Dinklage & Co Pharmacologically active quinazolinone compound, its use in pharmacological preparations and process for its manufacture

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3231572A (en) * 1963-08-05 1966-01-25 Miles Lab 3-substituted-4-quinazolones

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3879393A (en) * 1973-06-18 1975-04-22 Miles Lab Derivatives of 1,3-disubstituted 2,4(1h,3h)-quinazolinediones
DE4203050A1 (en) * 1992-02-04 1992-12-10 Heiko Delecate Combined low voltage solar with compressed air engine - can be operated with solar power or pneumatic motor or as hybrid combination of both
US8552015B2 (en) 2002-02-06 2013-10-08 Novartis Ag Quinazolinone derivatives and their use as CB agonists
WO2005123694A3 (en) * 2004-06-17 2006-04-13 Novartis Ag Quinazolinone compounds for the treatment of cough
US20080004296A1 (en) * 2004-06-17 2008-01-03 Christine Charman Organic Compounds

Also Published As

Publication number Publication date
SE378422B (en) 1975-09-01
CH531524A (en) 1972-12-15
GB1245316A (en) 1971-09-08
FR2020814A1 (en) 1970-07-17
FR2020814B1 (en) 1974-02-01
FI52725B (en) 1977-08-01
DE1803210A1 (en) 1970-05-14
FI52725C (en) 1977-11-10

Similar Documents

Publication Publication Date Title
DE60034240T2 (en) DRUGS FOR THE TREATMENT OF MALIGNER TUMORS
JPS6089474A (en) Morphinan derivative, production thereof and antitumor agent containing said compound
DE2258561A1 (en) BASIC SUBSTITUTED PYRIMIDONE (4) DERIVATIVES, THE PROCESS FOR THEIR PRODUCTION AND THE MEDICINAL PRODUCTS CONTAINING THEM
EP0005828A1 (en) New substituted phenylpiperazine derivatives, pharmaceutical compositions containing them and process for their preparation
US3652567A (en) Quinazolinone derivative and process for the production thereof
US4025625A (en) Imidazothiazines
US3781431A (en) Benzomorphan derivatives as analgesic agents
US3172811A (en) Quinolone proteus infection treatment
US3888983A (en) Derivatives of thiazolino-pyrimidin-6-ones, in inducing analgesia
US3337539A (en) Tetraethoxy-1, 2, 3, 4-tetrahydroisoquinoline derivatives and salts thereof
US3435041A (en) 2-anilinoquinolines
US3536711A (en) 8-acylamino- and 8-carbalkoxyaminopurines
JPS6333365A (en) 1-substituted-3-aryl-7-chloro-3,4-dihydro(2h)- acridone n-oxide
JPH10507446A (en) Bis-2-aminopyridines, methods for their production and their use for controlling parasite infection
US3426017A (en) Sulfonylurea compounds
IE44886B1 (en) Quinoline carboxylic acid esters
US3515787A (en) Compositions and methods for producing a muscle relaxing effect in an animal with 2,3 - substituted - 6 - amino-4-quinazolones
US3329569A (en) Hypotensive compositions and methods of producing hypotension
FR2473522A1 (en) NOVEL DIHYDRO-2,3 IMIDAZO (1,2-B) PYRIDAZINE SUBSTITUTED DERIVATIVES AND MEDICAMENTS, PARTICULARLY USEFUL AS ANTIDEPRESSANTS, CONTAINING THEM
CN101092414A (en) Preparation and application of a category of 6 - aryl - 3 - cycroamido methyl pyrone derviation
Chien et al. Synthesis and antimalarial evaluation of some 1, 7-naphthridines and 2, 9-diazaanthracenes
SU1447283A3 (en) Method of producing condensed derivatives of as-triazine
US3535321A (en) 2-carbalkoxyaminodihydroquinazolines
NO123430B (en)
US3562280A (en) Substituted 1,2,3,4-tetrahydroisoquinolines