BE633582A - - Google Patents

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Publication number
BE633582A
BE633582A BE633582DA BE633582A BE 633582 A BE633582 A BE 633582A BE 633582D A BE633582D A BE 633582DA BE 633582 A BE633582 A BE 633582A
Authority
BE
Belgium
Prior art keywords
emi
hours
heated
reflux
toluene
Prior art date
Application number
Other languages
French (fr)
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.)
Publication of BE633582A publication Critical patent/BE633582A/fr

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D207/00Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
    • C07D207/02Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D207/30Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having two double bonds between ring members or between ring members and non-ring members
    • C07D207/34Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having two double bonds between ring members or between ring members and non-ring members 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 ring carbon atoms

Description

       

   <EMI ID=1.1> 

  
La présente invention se rapporte à des composés alkoxyphénylés comportant un cycle pyrrolique. Elle concerne plus p&rticu-

  
 <EMI ID=2.1> 

  

 <EMI ID=3.1> 


  
leurs sels et leurs esters alkyliques inférieurs., ainsi que des

  
 <EMI ID=4.1> 

  
 <EMI ID=5.1>   <EMI ID=6.1> 

  
faisant réagir des acides 6-aroyl-4-oxohexanolques de formule 

  

 <EMI ID=7.1> 


  
 <EMI ID=8.1> 

  
de formule : ' ... 

  
 <EMI ID=9.1> 

  
où Ar a la signification qui lui est donnée plus haut. La faction peut être exécutée dans un solvant inerte tel que le toluène, le

  
 <EMI ID=10.1> 

  
toluène est un solvant préféré. Lorsqu'un des réactifs est liquide

  
à la température de réaction, le procède peut être exécuté également sans solvant ajouté. Le mélange de réaction peut être additionné d'un

  
 <EMI ID=11.1> 

  
un excès modéré de l'un d'eux. La température à laquelle on effectue

  
 <EMI ID=12.1> 

  
 <EMI ID=13.1> 

  
 <EMI ID=14.1> 

  
ques minutes à plusieurs jours suivant la température et les réactifs' particuliers. En utilisant du toluène à la température de reflux, la 

  
 <EMI ID=15.1> 

  
Le produit peut être isolé "ou" la forme d'un acide carbo- 

  
 <EMI ID=16.1>   <EMI ID=17.1> 

  

 <EMI ID=18.1> 


  
 <EMI ID=19.1>  

  

 <EMI ID=20.1> 


  
 <EMI ID=21.1> 

  
où Ar a la signification oui lui a été donnée ci-dessus, suivie,

  
si on le désire, de transformation en sel ou en ester alkylicue inférieur.

  
Les produits de l'invention sont de précieux agents pharmacologiques et intermédiaires chimiques. Ce sont des agents hypocho-

  
 <EMI ID=22.1> 

  
de solubilité voulues.

  
L'invention est illustrée par les exemples suivants. 

  
 <EMI ID=23.1>  cristallisation dans l'éthanol aqueux.

  
 <EMI ID=24.1> 

  
 <EMI ID=25.1> 

  
 <EMI ID=26.1>   <EMI ID=27.1> 

  
 <EMI ID=28.1>  

  
 <EMI ID=29.1> 

  
L'ester éthylique est préparé d'une façon analogue en chauffant

  
 <EMI ID=30.1> 

  
 <EMI ID=31.1> 

  
chauffée au reflux pendant 22 heures en éliminant de façon continue l'eau formée dans le produit de condensation* Le mélange de réaction

  
 <EMI ID=32.1>  

  
 <EMI ID=33.1>   <EMI ID=34.1> 

  
 <EMI ID=35.1> 

  
xyde de sodium, et chauffé au reflux pendant 4 heures encore" La 

  
 <EMI ID=36.1> 

  
sépare est recueilli sur un filtre et lavé à l'eau; point de fusion

  
 <EMI ID=37.1> 

  
 <EMI ID=38.1> 

  
On reprend le procédé ci-dessus en remplaçant l'iodure

  
 <EMI ID=39.1> 

  
 <EMI ID=40.1> 

  
 <EMI ID=41.1> 

  
 <EMI ID=42.1> 

  
 <EMI ID=43.1> 

  
point de fusion 129-132[deg.]C.

  
 <EMI ID=44.1> 

  
89-90.C.. 

  
Le produit de départ peut t'obtenir de la façon suivante.

  
 <EMI ID=45.1> 

  
 <EMI ID=46.1> 

  
 <EMI ID=47.1>  

  
 <EMI ID=48.1> 

  
posé et environ 5 fois son poids d'une solution de 4 parties en volume d'éthanol par partie en volute d'acide chlorhydrique sont ensuite chauffés à l'ébullition pendant environ 5 heures ou jusqu'

  
 <EMI ID=49.1> 

  
lition avec de l'acide chlorhydrique aqueux à 10-12%. En variante, le composé et environ 5 fois son poids d'une solution de 2 parties en volume d'éthanol par partie en volume d'acide chlorhydrique sont chauffés à ébullition pendant environ 16 heures, l'éthanol est

  
chassé par distillation et le résidu est chauffé à l'ébullition avec un mélange de 4 parties d'eau, de 1 partie d'acide chlorhydri-

  
 <EMI ID=50.1> 

  
 <EMI ID=51.1> 

  
 <EMI ID=52.1> 

  
reflux pendant 19 heures, agitée avec du charbon, filtrée et diluée

  
 <EMI ID=53.1> 

  
pyrrole-2-propionique qui se sépare au refroidissement est recueilli

  
 <EMI ID=54.1> 

  
 <EMI ID=55.1> 

  
 <EMI ID=56.1> 

  
dant 18 heures en éliminant de façon continue l'eau forméedans le produit de condensation. Le mélange de réaction est refroidi e,.. 

  
 <EMI ID=57.1>  

  
 <EMI ID=58.1> 

  
ne est chauffée au reflux pendant 3 heures en éliminant de façon continue l'eau formée dans le produit de condensation. Le mélange est

  
 <EMI ID=59.1> 

  
role-2-propionique insoluble qui se sépare est recueilli et lavé

  
 <EMI ID=60.1> 

  
après cristallisation dans l'éthanol aqueux,

  
 <EMI ID=61.1> 

  
 <EMI ID=62.1> 

  
sulfonique dans 50 cm de toluène est chauffée au reflux pendant 5 heures en éliminant de façon continue l'eau formée dans le produit

  
 <EMI ID=63.1> 

  
est recueilli et lavé avec de l'éther de pétrole; point de fusion .

  
 <EMI ID=64.1> 



   <EMI ID = 1.1>

  
The present invention relates to alkoxyphenyl compounds comprising a pyrrolic ring. It concerns more p & rticu-

  
 <EMI ID = 2.1>

  

 <EMI ID = 3.1>


  
their salts and their lower alkyl esters, as well as

  
 <EMI ID = 4.1>

  
 <EMI ID = 5.1> <EMI ID = 6.1>

  
reacting 6-aroyl-4-oxohexanolques acids of the formula

  

 <EMI ID = 7.1>


  
 <EMI ID = 8.1>

  
of formula: '...

  
 <EMI ID = 9.1>

  
where Ar has the meaning given to it above. The faction can be performed in an inert solvent such as toluene,

  
 <EMI ID = 10.1>

  
toluene is a preferred solvent. When one of the reagents is liquid

  
at the reaction temperature, the process can also be carried out without added solvent. The reaction mixture can be added with

  
 <EMI ID = 11.1>

  
a moderate excess of any of them. The temperature at which

  
 <EMI ID = 12.1>

  
 <EMI ID = 13.1>

  
 <EMI ID = 14.1>

  
only minutes to several days depending on temperature and specific reagents. Using toluene at reflux temperature, the

  
 <EMI ID = 15.1>

  
The product can be isolated "or" in the form of a carbo-

  
 <EMI ID = 16.1> <EMI ID = 17.1>

  

 <EMI ID = 18.1>


  
 <EMI ID = 19.1>

  

 <EMI ID = 20.1>


  
 <EMI ID = 21.1>

  
where Ar has the meaning yes it was given above, followed,

  
if desired, conversion to a salt or a lower alkyl ester.

  
The products of the invention are valuable pharmacological agents and chemical intermediates. They are hypocho-

  
 <EMI ID = 22.1>

  
desired solubility.

  
The invention is illustrated by the following examples.

  
 <EMI ID = 23.1> crystallization from aqueous ethanol.

  
 <EMI ID = 24.1>

  
 <EMI ID = 25.1>

  
 <EMI ID = 26.1> <EMI ID = 27.1>

  
 <EMI ID = 28.1>

  
 <EMI ID = 29.1>

  
The ethyl ester is prepared in a similar fashion by heating

  
 <EMI ID = 30.1>

  
 <EMI ID = 31.1>

  
heated at reflux for 22 hours while continuously removing the water formed in the condensation product * The reaction mixture

  
 <EMI ID = 32.1>

  
 <EMI ID = 33.1> <EMI ID = 34.1>

  
 <EMI ID = 35.1>

  
sodium xide, and heated at reflux for a further 4 hours.

  
 <EMI ID = 36.1>

  
separates is collected on a filter and washed with water; Fusion point

  
 <EMI ID = 37.1>

  
 <EMI ID = 38.1>

  
The above process is repeated by replacing the iodide

  
 <EMI ID = 39.1>

  
 <EMI ID = 40.1>

  
 <EMI ID = 41.1>

  
 <EMI ID = 42.1>

  
 <EMI ID = 43.1>

  
melting point 129-132 [deg.] C.

  
 <EMI ID = 44.1>

  
89-90.C ..

  
The starting material can get you in the following way.

  
 <EMI ID = 45.1>

  
 <EMI ID = 46.1>

  
 <EMI ID = 47.1>

  
 <EMI ID = 48.1>

  
placed and about 5 times its weight of a solution of 4 parts by volume of ethanol per part by volume of hydrochloric acid are then heated to the boil for about 5 hours or until

  
 <EMI ID = 49.1>

  
lition with 10-12% aqueous hydrochloric acid. Alternatively, the compound and about 5 times its weight of a solution of 2 parts by volume of ethanol per part by volume of hydrochloric acid are heated to a boil for about 16 hours, the ethanol is

  
removed by distillation and the residue is heated to boiling with a mixture of 4 parts of water, 1 part of hydrochloric acid.

  
 <EMI ID = 50.1>

  
 <EMI ID = 51.1>

  
 <EMI ID = 52.1>

  
reflux for 19 hours, stirred with charcoal, filtered and diluted

  
 <EMI ID = 53.1>

  
pyrrole-2-propionic which separates on cooling is collected

  
 <EMI ID = 54.1>

  
 <EMI ID = 55.1>

  
 <EMI ID = 56.1>

  
for 18 hours by continuously removing the water formed in the condensation product. The reaction mixture is cooled to ..

  
 <EMI ID = 57.1>

  
 <EMI ID = 58.1>

  
is heated under reflux for 3 hours while continuously removing the water formed in the condensation product. The mixture is

  
 <EMI ID = 59.1>

  
insoluble role-2-propionic acid which separates is collected and washed

  
 <EMI ID = 60.1>

  
after crystallization from aqueous ethanol,

  
 <EMI ID = 61.1>

  
 <EMI ID = 62.1>

  
sulfonic acid in 50 cm of toluene is heated under reflux for 5 hours while continuously removing the water formed in the product

  
 <EMI ID = 63.1>

  
is collected and washed with petroleum ether; Fusion point .

  
 <EMI ID = 64.1>


    

Claims (1)

<EMI ID=65.1> <EMI ID = 65.1> . acétique glacial est chauffée au reflux pendant 6 heures et diluée avec 50 d'eau chaude. Le mélange est refroidi et l'acide 1- <EMI ID=66.1> . glacial acetic acid is heated under reflux for 6 hours and diluted with 50% hot water. The mixture is cooled and the acid 1- <EMI ID = 66.1> <EMI ID=67.1> <EMI ID = 67.1> <EMI ID=68.1> <EMI ID=69.1> <EMI ID = 68.1> <EMI ID = 69.1> <EMI ID=70.1> <EMI ID = 70.1> et leurs sois et esters alkyliques inférieurs; où Ar représente and their sois and lower alkyl esters; where Ar represents <EMI ID=71.1> <EMI ID = 71.1> 7.- Procédé de préparation de composés de formule <EMI ID=72.1> <EMI ID=73.1> 7.- Process for the preparation of compounds of formula <EMI ID = 72.1> <EMI ID = 73.1> <EMI ID=74.1> <EMI ID = 74.1> <EMI ID=75.1> <EMI ID = 75.1> <EMI ID=76.1> <EMI ID = 76.1> <EMI ID=77.1> <EMI ID = 77.1> <EMI ID=78.1> <EMI ID = 78.1> <EMI ID=79.1> <EMI ID = 79.1> <EMI ID=80.1> <EMI ID = 80.1> <EMI ID=81.1> <EMI ID = 81.1> <EMI ID=82.1> <EMI ID = 82.1> <EMI ID=83.1> <EMI ID=84.1> <EMI ID = 83.1> <EMI ID = 84.1> <EMI ID=85.1> <EMI ID = 85.1> <EMI ID=86.1> <EMI ID = 86.1>
BE633582D 1963-06-13 BE633582A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR937998A FR1360529A (en) 1963-06-13 1963-06-13 New aryl compounds and processes for preparing these compounds

Publications (1)

Publication Number Publication Date
BE633582A true BE633582A (en)

Family

ID=8805984

Family Applications (1)

Application Number Title Priority Date Filing Date
BE633582D BE633582A (en) 1963-06-13

Country Status (2)

Country Link
BE (1) BE633582A (en)
FR (1) FR1360529A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5935990A (en) * 1996-12-10 1999-08-10 G.D. Searle & Co. Substituted pyrrolyl compounds for the treatment of inflammation

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1271082A (en) * 1968-05-07 1972-04-19 Wyeth John & Brother Ltd Furan, pyrrole and thiophene derivatives

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5935990A (en) * 1996-12-10 1999-08-10 G.D. Searle & Co. Substituted pyrrolyl compounds for the treatment of inflammation

Also Published As

Publication number Publication date
FR1360529A (en) 1964-05-08

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