Sodium Carbonate → HCID 23687033, Verbindung

HRID 727437

Reaktionsgleichung

Reaktionsgleichung von HRID 727437
[NH2:1][C:2]1[C:7](I)=[CH:6][C:5]([Br:9])=[CH:4][C:3]=1[S:10]([OH:13])(=[O:12])=[O:11].[CH:14]([C:16]1[CH:17]=[C:18](B(O)O)[CH:19]=[CH:20][CH:21]=1)=[O:15].C(=O)([O-])[O-].[Na+:29].[Na+]>CN(C)C=O.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[NH2:1][C:2]1[C:3]([S:10]([O-:13])(=[O:12])=[O:11])=[CH:4][C:5]([Br:9])=[CH:6][C:7]=1[C:20]1[CH:19]=[CH:18][CH:17]=[C:16]([CH:14]=[O:15])[CH:21]=1.[Na+:29]

Komponenten

7

Edukt 3

HCID 10340Sodium CarbonateHCID 27343563-Formylphenylboronic acidHCID 189193852-Amino-5-bromo-3-iodobenzenesulphonic acid

Produkt 1

HCID 23687033HCID 23687033, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418397HCID 178418397, VerbindungKatalysatorHCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of 11.34 g (30 mmol) of 2-amino-5-bromo-3-iodobenzenesulphonic acid, 4.5 g (30 mmol) of 3-formylbenzeneboronic acid, 10.5 g (99 mmol) of sodium carbonate and 1.73 g (1.5 mmol) of tetrakis(triphenylphosphine)palladium (0) in 40 ml of dimethylformamide and 20 ml of water is heated at 70° C. under argon for 5 hours. The reaction medium is then concentrated under reduced pressure and the residue is purified by chromatography on an RP 18 column, eluting with a water-acetonitrile mixture (8:2).

Aufarbeitung

  1. concentrationThe reaction medium is then concentrated under reduced pressure
  2. customthe residue is purified by chromatography on an RP 18 column
  3. washeluting with a water-acetonitrile mixture (8:2)

Quellen und Nachweise

ORD-Eintrag
ord-92a8fa4b0e33450eab77cc719d12fa31
Quelldatensatz
uspto-grants-1998_01
Patentnummer
US05712393

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