Diethyl (benzylamino)methylphosphonate → Diethyl (aminomethyl)phosphonate

HRID 45644Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 45644
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

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-4510b880f27d4920bce8c3650cf569ec
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08541448B2

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