CH280370A - Process for the preparation of a substance which lowers the level of prothrombin in the blood. - Google Patents

Process for the preparation of a substance which lowers the level of prothrombin in the blood.

Info

Publication number
CH280370A
CH280370A CH280370DA CH280370A CH 280370 A CH280370 A CH 280370A CH 280370D A CH280370D A CH 280370DA CH 280370 A CH280370 A CH 280370A
Authority
CH
Switzerland
Prior art keywords
lowers
blood
substance
prothrombin
level
Prior art date
Application number
Other languages
German (de)
Inventor
Podnik Spojene Farmace Narodni
Original Assignee
Spojene Farmaceuticke Z Narodn
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 Spojene Farmaceuticke Z Narodn filed Critical Spojene Farmaceuticke Z Narodn
Priority claimed from GB3687646A external-priority patent/GB632805A/en
Publication of CH280370A publication Critical patent/CH280370A/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/42Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms in positions 2 and 4
    • C07D311/44Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms in positions 2 and 4 with one hydrogen atom in position 3
    • C07D311/46Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms in positions 2 and 4 with one hydrogen atom in position 3 unsubstituted in the carbocyclic ring
    • C07D311/48Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms in positions 2 and 4 with one hydrogen atom in position 3 unsubstituted in the carbocyclic ring with two such benzopyran radicals linked together by a carbon chain

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

  

  Verfahren zur Herstellung einer das     Prothrombinniveau    im Blut  herabsetzenden Substanz.    Gegenstand der Erfindung ist ein Verfah  ren zur Herstellung einer das     Prothrombin-          niveau    im Blut herabsetzenden Substanz,     wel-          ehes    dadurch gekennzeichnet ist, dass eine Ver  bindung der Formel  
EMI0001.0006     
    mit einer Verbindung der Formel       (CFI3)2CH    . Y,  wobei X und Y reaktionsfähige, bei der Reak  tion mit Ausnahme eines in einem von ihnen  enthaltenen Sauerstoffatoms sieh abspaltende  Reste bedeuten, umgesetzt wird.

   Der so erhal  tene Bis-     (4-oxy-cumarinyl)-essigsäure-isopro-          pylester    bildet farblose, in Wasser unlösliche  Kristalle vom Schmelzpunkt 204 bis 205  C.  



  Die Einführung der     Isopropylgruppe    ohne  gleichzeitige     Veresterung    der     Hydroxylgrup-          pen    in den     Oxycumarinresten    erfolgt zweck  mässig durch Behandlung der     Carbonsäure    mit       Isopropanol    in Gegenwart eines wasserentzie  henden Mittels, wie von trockenem Chlorwas  serstoff oder konzentrierter Schwefelsäure.    <I>Beispiel:</I>  70 g Bis-     (4-oxy-cumarinyl)-essigsäure    wur  den in 600     em3        3n-isopropanolischer    Salzsäure  suspendiert und unter Umrühren etwa fünf  Stunden am     Rückflusskühler    erhitzt.

   Der nach  Abkühlung des Reaktionsgutes auskristalli  sierte Ester wurde abgesaugt, mit Äther aus  gewaschen und getrocknet; Ausbeute 62 g.  Nach     Umkristallisieren    aus Aceton zeigte das  gereinigte Produkt den Schmelzpunkt 204 bis  205  C.



  Process for the preparation of a substance which lowers the level of prothrombin in the blood. The subject matter of the invention is a method for producing a substance which lowers the prothrombin level in the blood, which is characterized in that a compound of the formula
EMI0001.0006
    with a compound of the formula (CFI3) 2CH. Y, where X and Y are reactive, in the reaction with the exception of an oxygen atom contained in one of them means separating radicals, is implemented.

   The bis (4-oxy-coumarinyl) -acetic acid isopropyl ester obtained in this way forms colorless, water-insoluble crystals with a melting point of 204 to 205 C.



  The introduction of the isopropyl group without simultaneous esterification of the hydroxyl groups in the oxycoumarin residues is expediently carried out by treating the carboxylic acid with isopropanol in the presence of a dehydrating agent such as dry hydrogen chloride or concentrated sulfuric acid. <I> Example: </I> 70 g of bis- (4-oxy-coumarinyl) -acetic acid were suspended in 600 cubic meters of 3N-isopropanolic hydrochloric acid and heated on the reflux condenser for about five hours while stirring.

   The ester crystallized out after the reaction mixture had cooled down was filtered off with suction, washed off with ether and dried; Yield 62g. After recrystallization from acetone, the purified product had a melting point of 204 to 205 C.

 

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung einer das Pro- thrombinniveau im Blut herabsetzenden Sub stanz, dadurch gekennzeichnet, dass eine Ver bindung der Formel EMI0001.0024 mit einer Verbindung der Formel (CH3) 2CH . Y, wobei X und Y reaktionsfähige, bei der Reak tion mit Ausnahme eines in einem von ihnen enthaltenen Sauerstoffatoms sich abspaltende Reste bedeuten, umgesetzt wird. Der so erhal tene Bis-(4-oxy-cumarinyl)-essigsäure-isopro- pylester bildet farblose, in Wasser unlösliche Kristalle vom Schmelzpunkt 204 bis 205 C. PATENT CLAIM: Process for the production of a substance which lowers the prothrombin level in the blood, characterized in that a compound of the formula EMI0001.0024 with a compound of the formula (CH3) 2CH. Y, where X and Y are reactive radicals which are split off in the reaction with the exception of an oxygen atom contained in them, is implemented. The bis (4-oxy-coumarinyl) -acetic acid isopropyl ester obtained in this way forms colorless, water-insoluble crystals with a melting point of 204 to 205 C. UNTERANSPRUCH: Zerfahren nach Patentanspruch, dadurch gekennzeichnet, dass Bis- (I-oxy-cumarinyl)- essigsäure mit Isopropanol in Gegenwart eines wasserentziehenden Mittels am Rüekflussküh- ler behandelt wird und das nach Erkalten des Reaktionsgattes auskristallisierte Produkt ab filtriert, mit einem organischen Lösungsmittel gewaschen und getrocknet wird. SUBSTANTIAL CLAIM: Process according to patent claim, characterized in that bis- (I-oxy-coumarinyl) - acetic acid is treated with isopropanol in the presence of a dehydrating agent on the reflux cooler and the product which crystallizes out after the reaction gate has cooled down is filtered off and washed with an organic solvent and is dried.
CH280370D 1946-08-31 1946-11-06 Process for the preparation of a substance which lowers the level of prothrombin in the blood. CH280370A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CS2482512X 1946-08-31
CH280370T 1946-11-06
GB3687646A GB632805A (en) 1946-12-13 1946-12-13 Process for the production of compounds reducing the prothrombin level in the blood

Publications (1)

Publication Number Publication Date
CH280370A true CH280370A (en) 1952-01-15

Family

ID=32233754

Family Applications (1)

Application Number Title Priority Date Filing Date
CH280370D CH280370A (en) 1946-08-31 1946-11-06 Process for the preparation of a substance which lowers the level of prothrombin in the blood.

Country Status (1)

Country Link
CH (1) CH280370A (en)

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