Hydrogen Peroxide → HCID 10298064, compound

Participants

Reaction Steps

To a solution of 40 mg (0.91 mmol) of 3-[(1-ethyl-7,8-dimethoxy-2-oxo-5-phenyl-2,3-dihydro-1H-1,4-benzodiazepin-3-yl)methyl]benzonitrile (IIcp) in 1 ml of ethanol, add under an inert atmosphere 27 μl (0.27 mmol) of 30% (m/m) H2O2 in water, 36 μl (0.018 mmol) of 0.5 M NaOH in water. Stir under reflux for 12 hours. Evaporate to dryness. Take up in a 25 ml of a water-ice mixture. Filter the solid, wash twice with 20 ml of water and once with 5 ml of ether. One obtains 24 mg of the abovenamed product as a white powder. Yield: 59%. M: 111–113° C. 1H-NMR (CDCl3, 200 MHz): d 1.10 (s, 3H, CH3), 3.50–3.75 (m, 6H, 1H —CH2Ph+1H —NCH2+CH+OCH3), 3.98–4.11 (m, 4H, 1H —CH2Ph+OCH3), 4.38–4.49 (m, 1H —NCH2), 5.91 (m, 1H exchangeable CO—NH2), 6.26 (m, 1H exchangeable CO—NH2), 6.66 (s, 1H Ar), 6.85 (s, 1H Ar), 7.30–7.86 (m, 9H Ar).

Provenance & Evidence