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GB1308370A - 1-hydroxy-3-oxo-benzimidazoles quinoxaline-di-n-oxides and benzimidazole-mono-and di-n-oxides - Google Patents

1-hydroxy-3-oxo-benzimidazoles quinoxaline-di-n-oxides and benzimidazole-mono-and di-n-oxides

Info

Publication number
GB1308370A
GB1308370A GB4720270A GB4720270A GB1308370A GB 1308370 A GB1308370 A GB 1308370A GB 4720270 A GB4720270 A GB 4720270A GB 4720270 A GB4720270 A GB 4720270A GB 1308370 A GB1308370 A GB 1308370A
Authority
GB
United Kingdom
Prior art keywords
alkali metal
alkyl
benzimidazole
quinoxaline
oxides
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
Application number
GB4720270A
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.)
Research Corp
Original Assignee
Research Corp
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
Priority claimed from US04/883,577 external-priority patent/US4343942A/en
Application filed by Research Corp filed Critical Research Corp
Publication of GB1308370A publication Critical patent/GB1308370A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D235/00Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
    • C07D235/02Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D235/00Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
    • C07D235/02Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
    • C07D235/04Benzimidazoles; Hydrogenated benzimidazoles
    • C07D235/22Benzimidazoles; Hydrogenated benzimidazoles with hetero atoms directly attached to ring nitrogen atoms
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D235/00Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
    • C07D235/02Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
    • C07D235/04Benzimidazoles; Hydrogenated benzimidazoles
    • C07D235/24Benzimidazoles; Hydrogenated benzimidazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D241/00Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings
    • C07D241/36Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings condensed with carbocyclic rings or ring systems
    • C07D241/38Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings condensed with carbocyclic rings or ring systems with only hydrogen or carbon atoms directly attached to the ring nitrogen atoms
    • C07D241/40Benzopyrazines
    • C07D241/44Benzopyrazines with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to carbon atoms of the hetero ring
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D241/00Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings
    • C07D241/36Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings condensed with carbocyclic rings or ring systems
    • C07D241/50Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings condensed with carbocyclic rings or ring systems with hetero atoms directly attached to ring nitrogen atoms
    • C07D241/52Oxygen atoms

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Plural Heterocyclic Compounds (AREA)

Abstract

1308370 Quinoxaline-di-N-oxides and benzimidazole-N-oxides RESEARCH CORP 5 Oct 1970 [9 Dec 1969] 47202/70 Addition to 1215815 Heading C2C Novel process for preparing quinoxaline-di- N-oxides and benzimidazole mono- and di- N-oxides which comprises reacting a compound having a methylene group activated by two electron-withdrawing groups, or a compound containing a methylene group which is activated by one electron-withdrawing group selected from nitro, carbonyl of a ketone or aldehyde, with an iosbenzofuroxan in the presence of a base, the activated methylene containing compound and bases being (a) a malonic acid diester in the presence of an alkali metal hydroxide or an alkali metal hydride; (b) a malonamate in 'the presence of alkali metal hydroxide, alkali 'metal alkoxide or alkali metal hydride; (c) a malonic acid diamide in the presence of a base; (d) #-keto ester in the presence of ammonia, a primary or secondary amine or an alkali metal hydride; (e) #-diketone in the presence of ammonia, a primary or secondary amine or alkali metal hydride; (f) #-keto amide in the presence of a tertiary amine, an alkali metal hydroxide, and alkali metal alkoxide, or an alkali metal hydride; (g) a primary or secondary nitro compound in the presence of an alkali metal hydroxide, an alkali metal alkoxide or an alkali metal hydride; (h) malononitrile, cyanoacetamide or a cyano acetate with an alkali metal hydride; (i) a pyruvaldehyde acetal other than the dimethyl acetal in the presence of ammonia or a primary, secondary or tertiary amine; (j) an alicyclic ketone in the presence of alkali metal hydroxide, alkoxide or hydride; (k) a heterocyclic ketone in the presence of ammonia, primary, secondary or tertiary amine or an alkali metal hydroxide, alkoxide or hydride; (1) a ketosulphonyl compound or ketosulphonamide in the presence of a base ; or (m) a C 1-7 alkyl-γ-γ-di-(C 1-7 alkoxy)-acetoacetate other than ethyl-γ,γ-diethoxy acetoacetate in the presence of ammonia, a primary, secondary or tertiary amine or an alkali metal hydroxide, alkoxide or hydride. Novel compounds produced by the process are wherein X is fluoro, trifluoromethyl, sulphonamido, N-methyl sulphonamido or N,N-dimethylsulphonamido substituted on one or more positions of the benzene ring of the quinoxaline and each of R<SP>1</SP> and R<SP>11</SP> is hydrogen or C 1-7 alkyl; wherein R 6 is C 1-7 alkoxy, aryloxy, benzyloxy or NR 8 R 9 where R 8 and R 9 are hydrogen, C 1-7 alkyl, or phenyl; and X is hydrogen, chloro, fluoro, methyl, methoxy, trifluoromethyl, sulphonamido, N-methylsulphonamido or N, N-dimethylsulphonamido substituted on one or more positions of the benzene ring of the quinoxaline, excluding the compounds 2-carbomethoxy-3- hydroxy quinoxaline-di-N-oxide and 2-carboethoxy-3-hydroxy quinoline-di-N-oxide; where X is as in Formula XI where X and R 6 are as in Formula XII wherein X is as in Formula XII, R is C 1-7 alkyl and Y<SP>1</SP> is hydrogen, carbo-C 1-7 alkoxy, excluding 2-formyldimethyl-acetal quinoxaline di-N- oxide and 2-carboethoxy-3-formyl-diethyl acetalquinoxaline di-N-oxide; where X is as in Formula XII, R 4 is C 1-7 alkyl or phenyl and m is zero or 1; where X is as in Formula XII, Z is oxygen, sulphur imino or N-methylimino, m is zero or 1 and n is 2 or 3; where X is as in Formula XII, R 7 is C 1-7 alkyl and Z<SP>1</SP> is halogen, C 1-7 alkoxy, C 1-7 alkanoyloxy, cyano, phenoxy, amino, mercapto or C 1-7 alkylmercapto ; where X is as in Formula XII, R 11 and R 12 are each methyl or ethyl optionally substituted'with chloro, bromo, hydroxy or diethylamino or, taken with the carbon to which they are attached, are cyclohexyl, excluding 2,2-dimethyl- 2H-benzimidazole-1,3-dioxide and 2-methyl-2- ethyl-2H-benzimidazole-1,3-dioxide ; where X is as defined in XII and R 10 is hydrogen, optionally substituted alkyl or aryl, carbalkoxy, or carboxamido, excluding 1-hydroxy-2-benzimidazole propionamide-3-oxide and 1-hydroxy- 2-carbethoxy benzimidazole-3-oxide; where X is as defined in Formula XII, m is 2 to 16, R 3 is halogen, hydroxyl, alkoxy, acetoxy, alkyl, aryl, acetyl, amino, alkylamino, arylamino, acylamino, aroylamino, carboxy, carbalkoxy, nitrile or amido. Other known compounds may also be prepared by the process. Methyl γ,γ-diethoxyacetoacetate may be prepared by reaction of ethyl diethoxyacetate and methyl acetate in the presence of sodium, the former reactant being prepared by reaction of sodium ethoxide and dichloroacetic acid. Pharmaceutical compositions of the compounds of the process show antimicrobial activity when administered topically with the usual excipients and many of the compounds described show growth promotion activity in animals, control chronic respiratory disease in pultry, infectious sinusitis in turkeys, urinary-tract and systemic and non-systemic infections in animals. The compounds are also useful as industrial antimicrobials.
GB4720270A 1969-12-09 1970-10-05 1-hydroxy-3-oxo-benzimidazoles quinoxaline-di-n-oxides and benzimidazole-mono-and di-n-oxides Expired GB1308370A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US04/883,577 US4343942A (en) 1966-11-08 1969-12-09 Quinoxaline derivatives

Publications (1)

Publication Number Publication Date
GB1308370A true GB1308370A (en) 1973-02-21

Family

ID=25382881

Family Applications (1)

Application Number Title Priority Date Filing Date
GB4720270A Expired GB1308370A (en) 1969-12-09 1970-10-05 1-hydroxy-3-oxo-benzimidazoles quinoxaline-di-n-oxides and benzimidazole-mono-and di-n-oxides

Country Status (1)

Country Link
GB (1) GB1308370A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2527157A1 (en) * 1974-06-18 1976-02-05 Egyt Gyogyszervegyeszeti Gyar PROCESS FOR THE PREPARATION OF (QUINOXALINE-N HIGH 1, N HIGH 4-DIOXYDE-2-YLMETHYLENE) -CARBAZIC ACID METHYLESTER
US3997535A (en) * 1973-03-16 1976-12-14 Allen & Hanburys Limited Quinoxaline-2-carboxamidotetrazoles
US4228151A (en) 1976-05-03 1980-10-14 L'oreal Cosmetic composition for imparting to human skin a coloration resembling a natural tan
US4228283A (en) 1978-11-24 1980-10-14 Marxer S.P.A. Process for preparing pure 2-methyl-3-(β-hydroxyethylcarbamoyl)quinoxaline 1,4-di-N-oxide, and other compounds similar thereto
US4264600A (en) 1978-10-20 1981-04-28 Eli Lilly And Company Treatment of influenza with 2-estersubstituted-3,4-dihydro-3-oxoquinoxalines
FR2482963A1 (en) * 1980-05-23 1981-11-27 Egyt Gyogyszervegyeszeti Gyar NOVEL QUINOXALINE-1,4-DIOXIDE DERIVATIVES, THEIR PREPARATION METHODS AND VETERINARY USE COMPOSITIONS CONTAINING SAME
US4333931A (en) 1978-12-19 1982-06-08 Ciba-Geigy Corporation Method of combatting harmful microorganisms using quinoxaline compounds
EP0287806A1 (en) * 1987-04-13 1988-10-26 The Firestone Tire & Rubber Company Rubber compositions modified with hydroxy-benzimidazole oxides

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3997535A (en) * 1973-03-16 1976-12-14 Allen & Hanburys Limited Quinoxaline-2-carboxamidotetrazoles
DE2527157A1 (en) * 1974-06-18 1976-02-05 Egyt Gyogyszervegyeszeti Gyar PROCESS FOR THE PREPARATION OF (QUINOXALINE-N HIGH 1, N HIGH 4-DIOXYDE-2-YLMETHYLENE) -CARBAZIC ACID METHYLESTER
US4228151A (en) 1976-05-03 1980-10-14 L'oreal Cosmetic composition for imparting to human skin a coloration resembling a natural tan
US4264600A (en) 1978-10-20 1981-04-28 Eli Lilly And Company Treatment of influenza with 2-estersubstituted-3,4-dihydro-3-oxoquinoxalines
US4228283A (en) 1978-11-24 1980-10-14 Marxer S.P.A. Process for preparing pure 2-methyl-3-(β-hydroxyethylcarbamoyl)quinoxaline 1,4-di-N-oxide, and other compounds similar thereto
US4333931A (en) 1978-12-19 1982-06-08 Ciba-Geigy Corporation Method of combatting harmful microorganisms using quinoxaline compounds
FR2482963A1 (en) * 1980-05-23 1981-11-27 Egyt Gyogyszervegyeszeti Gyar NOVEL QUINOXALINE-1,4-DIOXIDE DERIVATIVES, THEIR PREPARATION METHODS AND VETERINARY USE COMPOSITIONS CONTAINING SAME
EP0287806A1 (en) * 1987-04-13 1988-10-26 The Firestone Tire & Rubber Company Rubber compositions modified with hydroxy-benzimidazole oxides

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Legal Events

Date Code Title Description
PS Patent sealed
429A Application made for amendment of specification (sect. 29/1949)
429H Application (made) for amendment of specification now open to opposition (sect. 29/1949)
429D Case decided by the comptroller ** specification amended (sect. 29/1949)
SPA Amended specification published
PE20 Patent expired after termination of 20 years