Hydrogen Peroxide → HCID 54539508, compound

Participants

Reaction Steps

To a solution of sulfide 6a (2.36 g, 10 mmol), Na2WO4 ·2 H2O (49.5 mg, 0.15 mmol), and H2SO4 (1 M, 68 μL) in methanol (10 mL) was added dropwise 30% H2O2 (2.6 mL) at room temperature under nitrogen maintaining the temperature at 38-45° C. The mixture was aged at ambient temperature for 3 h and cooled ~18° C. Sodium sulfite (20% aqueous solution, 2.6 mL) was added slowly with an external cooling to maintain the temperature below 20° C. After aged for 0.5 h the mixture was diluted with water (20 mL) and filtered. The solid was washed with water (2×10 mL) and dried in vacuo to give 2.55 g of 6b as a light yellow solid: IR (thin film) 1700 cm-1 ; 1H NMR (CDCl3, 300 MHz) δ 7.92 (2 H), 7.64 (1 H), 7.52 (2 H), 4.24 (2 H), 3.04 (3 H), 2.05 (3 H), and 1.30 (3 H); 13C NMR (CDCl3, 75.5 MHz) δ 167.88, 141.50, 139.76, 136.29, 131.87, 130.21, 127.45, 61.24, 44.45, 14.28, and 14.14.

Provenance & Evidence