Phosphate → HCID 14567294, Verbindung

HRID 443380Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 443380
[Cl:1][C:2]1[N:3]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:5]2[C:10]([C:11]=1[CH:12]=[O:13])=[CH:9][CH:8]=[CH:7][CH:6]=2.P([O-])([O-])([O-])=[O:21].[Mn]([O-])(=O)(=O)=O.[K+]>CC(C)=O>[Cl:1][C:2]1[N:3]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:5]2[C:10]([C:11]=1[C:12]([OH:21])=[O:13])=[CH:9][CH:8]=[CH:7][CH:6]=2

Komponenten

5

Edukt 3

HCID 1061PhosphateHCID 516875Potassium PermanganateHCID 145672483-Chloro-1-phenylisoquinoline-4-carbaldehyde

Produkt 1

HCID 14567294HCID 14567294, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

53.5 g 3-Chloro-1-phenyl-isoquinoline-4-aldehyde are suspended in 1.5 l of acetone and 500 ml of phosphate buffer of pH 7. At 40° C., 40 g of potassium permanganate are introduced portionwise within 2 hours and stirring is continued at this temperature for 2 hours. The excess potassium permanganate is destroyed with 10 g sodium hydrogenosulfite and the solution is concentrated to 500 ml and filtered. The filtrate is brought to pH 4 with concentrated hydrochloric acid followed by thorough extraction with acetic ester. Removal of the solvent in vacuo provides 41.1 g of 3-chloro-1-phenyl-isoquinoline-4 carboxylic acid having a melting point of 208° C.

Aufarbeitung

  1. customThe excess potassium permanganate is destroyed with 10 g sodium hydrogenosulfite
  2. concentrationthe solution is concentrated to 500 ml
  3. filtrationfiltered
  4. extractionfollowed by thorough extraction with acetic ester
  5. customRemoval of the solvent in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7d023e8192de49ca9356f754fa684acb
Quelldatensatz
uspto-grants-1981_04
Patentnummer
US04260611

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