Sodium borohydride → HCID 22097164, Verbindung

HRID 861451Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 861451
[C:1]([NH:4][C:5]1[C:10]([NH:11][C:12](=[O:14])[CH3:13])=[CH:9][C:8]([Cl:15])=[C:7]([N+:16]([O-])=O)[CH:6]=1)(=[O:3])[CH3:2].[BH4-].[Na+]>C(O)C.O.S([O-])([O-])(=O)=O.[Cu+2]>[C:1]([NH:4][C:5]1[C:10]([NH:11][C:12](=[O:14])[CH3:13])=[CH:9][C:8]([Cl:15])=[C:7]([NH2:16])[CH:6]=1)(=[O:3])[CH3:2]

Komponenten

6

Edukt 2

HCID 4311764Sodium borohydrideHCID 22097084HCID 22097084, Verbindung

Produkt 1

HCID 22097164HCID 22097164, VerbindungAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 24462Copper SulfateKatalysatorHCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 4 g (14.7 mmol) of 4,5-diacetamido-1-chloro-2-nitrobenzene in 200 ml of ethanol were added a solution of 0.4 g of copper(II) sulfate×5H2O in 2 ml of water and subsequently, a little at a time, 1.1 g (29.4 mmol) of sodium borohydride. The mixture was refluxed for 3 hours and subsequently filtered. The filtrate was concentrated, and the crude product was washed with water and methylene chloride. Workup of the organic phase gave a yield of 94% of the product. Melting point 237° C.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 3 hours
  2. filtrationsubsequently filtered
  3. concentrationThe filtrate was concentrated
  4. washthe crude product was washed with water and methylene chloride

Quellen und Nachweise

ORD-Eintrag
ord-e899707c5b1846e480516f6e2cee07bd
Quelldatensatz
uspto-grants-1998_02
Patentnummer
US05714489

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