Water → HCID 178487711, Verbindung

HRID 420082

Reaktionsgleichung

Reaktionsgleichung von HRID 420082
Cl[C:2]1[C:11]2[C:6](=[C:7]([Cl:14])[C:8]([O:12][CH3:13])=[CH:9][CH:10]=2)[N:5]=[C:4]([N:15]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[N:16]2)[CH:3]=1.CC(O[K])=[O:26].O>CS(C)=O>[Cl:14][C:7]1[C:8]([O:12][CH3:13])=[CH:9][CH:10]=[C:11]2[C:6]=1[N:5]=[C:4]([N:15]1[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[N:16]1)[CH:3]=[C:2]2[OH:26]

Komponenten

5

Edukt 3

HCID 962Water2×HCID 56605213HCID 56605213, VerbindungHCID 178476685HCID 178476685, Verbindung

Produkt 1

HCID 178487711HCID 178487711, VerbindungAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

To a solution of compound 119b (250 mg) in DMSO (2.5 mL) was added CH3COOK (3 eq.), water (2 eq.). The reaction mixture was heated to 140° C. for 4 hrs. After cooled to RT, water (1 mL) was added to the reaction mixture slowly under stirring. Solid was filtered and washed with water to yield compound 88b in >80% yield. In a separate reaction, when 5 eq. of CH3COOK was used, the reaction was completed in 1 hr.

Aufarbeitung

  1. temperatureAfter cooled to RT
  2. filtrationSolid was filtered
  3. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-dc9bd193c5ad415e9613025dfc85b1ff
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08093379B2

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