Ammonium Chloride → HCID 54401849, Verbindung

HRID 1378967Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1378967
[CH2:1]([O:3][P:4]([CH:9]=[CH:10][C:11]1[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][CH:12]=1)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[Cl-].[NH4+]>[Fe]>[CH2:6]([O:5][P:4]([CH:9]=[CH:10][C:11]1[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=1)(=[O:8])[O:3][CH2:1][CH3:2])[CH3:7]

Komponenten

4

Edukt 2

HCID 25517Ammonium ChlorideHCID 53749636Diethyl [2-(4-nitrophenyl)ethenyl]phosphonate

Produkt 1

HCID 54401849HCID 54401849, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 23925IronKatalysator

Versuchsvorschrift

A suspension containing 4-nitrostyrylphosphonic acid diethyl ester (3.0 g, 10.5 mmol), iron powder (5.58 g, 100 mmol) and ammonium chloride (5.58 g, 104 mmol) is heated to reflux for 45 minutes. The reaction medium is filtered through Celite. The filtrate is concentrated under vacuum and is bipartitioned in a water/dichloromethane mixture. The organic phase is washed with water, then dried (MgSO4) and evaporated under vacuum to give the expected product, which crystallizes gradually.

Aufarbeitung

  1. temperatureis heated
  2. temperatureto reflux for 45 minutes
  3. filtrationThe reaction medium is filtered through Celite
  4. concentrationThe filtrate is concentrated under vacuum
  5. washThe organic phase is washed with water
  6. dry with materialdried (MgSO4)
  7. customevaporated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-1d84d78604e14006bc7cc888c2d45c30
Quelldatensatz
uspto-grants-1997_09
Patentnummer
US05670493

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