Diethyl (benzylamino)methylphosphonate → Diethyl (aminomethyl)phosphonate

HRID 870136Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 870136
C([NH:8][CH2:9][P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])C1C=CC=CC=1>C(O)C.C(O)(=O)C.[C].[Pd]>[NH2:8][CH2:9][P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13]

Komponenten

5

Edukt 1

HCID 10923173Diethyl (benzylamino)methylphosphonate

Produkt 1

HCID 1596920Diethyl (aminomethyl)phosphonate

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 176Acetic AcidLösungsmittelHCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A 250-mL pressure tank reactor was purged, flushed and maintained with a hydrogen atmosphere, then, was added a solution of diethyl (benzylamino)methylphosphonate (3.5 g, 13.62 mmol, 1.00 equiv) in ethanol (180 mL), acetic acid (10 mL) and Palladium carbon (0.2 g, 0.10 equiv). The resulting solution was stirred for 24 h at 50° C. under 20 atm pressure. The solids were filtered out. The resulting mixture was concentrated under vacuum. This resulted in 2.0 g (crude) of the title compound as brown oil which was used without further purification.

Aufarbeitung

  1. customA 250-mL pressure tank reactor was purged
  2. customflushed
  3. temperaturemaintained with a hydrogen atmosphere
  4. filtrationThe solids were filtered out
  5. concentrationThe resulting mixture was concentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-ee3306a6d62b48dc884c95f95a73112f
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969377B2

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