Potassium Carbonate → HCID 178472848, Verbindung

HRID 59618

Reaktionsgleichung

Reaktionsgleichung von HRID 59618
[CH2:1]([O:3][C:4](=[O:20])[C:5](=[N:9][NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13](Br)[C:12]=1[O:18][CH3:19])[C:6](=[O:8])[CH3:7])[CH3:2].[C:21]([C:24]1[CH:25]=[C:26](B(O)O)[CH:27]=[CH:28][CH:29]=1)([OH:23])=[O:22].C(=O)([O-])[O-].[K+].[K+]>C(O)C.O.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl>[CH2:1]([O:3][C:4]([C:5](=[N:9][NH:10][C:11]1[C:12]([O:18][CH3:19])=[C:13]([C:28]2[CH:27]=[CH:26][CH:25]=[C:24]([C:21]([OH:23])=[O:22])[CH:29]=2)[CH:14]=[CH:15][CH:16]=1)[C:6](=[O:8])[CH3:7])=[O:20])[CH3:2]

Komponenten

7

Edukt 3

HCID 11430Potassium CarbonateHCID 27339573-Carboxyphenylboronic acidHCID 178472845HCID 178472845, Verbindung

Produkt 1

HCID 178472848HCID 178472848, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6102075Dichlorobis(triphenylphosphine)palladiumKatalysatorHCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of ethyl-2-[(3-bromo-2-methoxyphenyl)hydrazono]-3-oxobutanoate (4 g) prepared as in Example 1, 3-carboxyphenylboronic acid (2.30 g), bis(triphenylphosphine)palladium(II)chloride [PdCl2(PPh3)2] (0.30 g), potassium carbonate (4.023 g) in ethanol (100 mL) and water (30 mL) was heated to about reflux temperature and stirred for about 20 hours. The hot mixture was filtered to remove the catalyst. The clear filtrate was concentrated under vacuum. To the residue, water (100 mL) was added, acidified to pH 3-5 using hydrochloric acid and stirred for about 30 minutes at about room temperature. The slurry was filtered, washed with water (25 ml) and dried in an oven at about 55° C. to about 60° C. for about 12 hours.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto about reflux temperature
  3. filtrationThe hot mixture was filtered
  4. customto remove the catalyst
  5. concentrationThe clear filtrate was concentrated under vacuum
  6. additionTo the residue, water (100 mL) was added
  7. stirringstirred for about 30 minutes at about room temperature
  8. filtrationThe slurry was filtered
  9. washwashed with water (25 ml)
  10. customdried in an oven at about 55° C. to about 60° C. for about 12 hours

Quellen und Nachweise

ORD-Eintrag
ord-c95f0e84387547e9947c0b711a65092a
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09440927B2

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