1,3,5-trimethoxy-2,4-dinitrobenzene → HCID 23009735, Verbindung

HRID 359638Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 359638
[N+:1]([C:4]1[C:9]([O:10][CH3:11])=[C:8]([N+:12]([O-])=O)[C:7]([O:15][CH3:16])=[CH:6][C:5]=1[O:17][CH3:18])([O-:3])=[O:2].[PH2]([O-])=O.[Na+]>[Pd].O1CCCC1.O>[NH2:12][C:8]1[C:9]([O:10][CH3:11])=[C:4]([N+:1]([O-:3])=[O:2])[C:5]([O:17][CH3:18])=[CH:6][C:7]=1[O:15][CH3:16]

Komponenten

6

Edukt 2

HCID 27749591,3,5-trimethoxy-2,4-dinitrobenzeneHCID 178527019HCID 178527019, Verbindung

Produkt 1

HCID 23009735HCID 23009735, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysatorHCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A suspension of 26 g of palladium on charcoal (10%) is refluxed in 1.3 l of tetrahydrofuran and 26 ml of water containing 1 mole (258 g) of 2,4-dinitro-1,3,5-trimethoxybenzene. A solution of 247 g of sodium hypophosphite in 260 ml of water is added to this suspension over 3 hours. Refluxing is continued for an additional 30 minutes. After cooling, the catalyst is removed by filtration and the aqueous phase by phase separation. The organic phase is concentrated under vacuum and is then poured onto ice. The expected product precipitates. It melts at 111° C.

Aufarbeitung

  1. temperatureRefluxing
  2. temperatureAfter cooling
  3. customthe catalyst is removed by filtration
  4. customthe aqueous phase by phase separation
  5. concentrationThe organic phase is concentrated under vacuum
  6. additionis then poured onto ice
  7. customThe expected product precipitates

Quellen und Nachweise

ORD-Eintrag
ord-53212ae6178b46fab4b2a15b4a3f3c7b
Quelldatensatz
uspto-grants-1991_03
Patentnummer
US05002585

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