Reaktion #640575

ord-279427bedc5d4d239b00cc6dfc2c8131

Reaktionsgleichung

O=C1OC(c2ccccc2)CCN1Cc1ccccc1[N+](=O)[O-]
3-(2-Nitrobenzyl)-6-phenyl-[1,3]-oxazinan-2-one
[Cl-].[NH4+]
ammonium chloride
O
water
Nc1ccccc1CN1CCC(c2ccccc2)OC1=O
3-(2-aminobenzyl)-6-phenyl-[1,3]-oxazinan-2-one
Ausbeute 99.3%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto reflux for 1.5 hours
  2. 2
    Filtrationthe reaction mixture was filtered with suction
  3. 3
    Extraktionextracted with ethyl acetate
  4. 4
    WaschenThe organic layer was washed with a saturated brine
  5. 5
    Trocknendried over anhydrous sodium sulfate

Vorschrift

3-(2-Nitrobenzyl)-6-phenyl-[1,3]-oxazinan-2-one (1.59 g, 5.10 mmol), iron powder (1.42 g, 25.4 mmol), ammonium chloride (0.14 g, 2.62 mmol) were suspended in ethanol (30 ml) and water (15 ml) and heated to reflux for 1.5 hours. After cooling to room temperature, the reaction mixture was filtered with suction and extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and 3-(2-aminobenzyl)-6-phenyl-[1,3]-oxazinan-2-one (1.43 g) was obtained by evaporating the solvent under reduced pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08048825B2uspto-grants-2011_11