Acetic Acid → HCID 178426257, Verbindung

HRID 1470225Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1470225
[CH3:1][C:2]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]3[N-:14][N:15]=[N:16][N:17]=3)[C:11](=[O:12])[N:6]2[CH:5]=[CH:4][CH:3]=1.[K+].C(O)(=O)C>O.C1COCC1>[CH3:1][C:2]1[C:7]2=[N:8][CH:9]=[C:10]([C:13]3[NH:14][N:15]=[N:16][N:17]=3)[C:11](=[O:12])[N:6]2[CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 2

HCID 176Acetic Acid3×HCID 443866Pemirolast potassium

Produkt 1

HCID 178426257HCID 178426257, VerbindungAusbeute 55,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

The free acid was prepared from pemirolast potassium (15.8 g; Chemtronica AB) by dissolution in a mixture of water (100 mL) and THF (80 mL) at room temperature and acidification with acetic acid (1 eq.; 17.5 g; 20% aq.). Firstly, ca. 1 mL of acetic acid was added and the obtained thin slurry was equilibrated for about 30 minutes. Thereafter the rest of the acetic acid was added slowly. The resultant thick slurry was diluted with water (50 mL) and equilibrated for 2 hours and then filtered and washed with water. The resultant solid was dried at 40° C. and under reduced pressure for 5-10 hours to yield 7.5 g of sub-title compound.

Aufarbeitung

  1. waitequilibrated for 2 hours
  2. filtrationfiltered
  3. washwashed with water
  4. customThe resultant solid was dried at 40° C. and under reduced pressure for 5-10 hours

Quellen und Nachweise

ORD-Eintrag
ord-f921b390e5bf453ead57fc367ec01415
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09006431B2

Notizen zur Reaktion

Wird geladen…