反应详情

A 50 L three-necked round bottom flask equipped with a mechanical stirrer, a 2 L dropping funnel, a nitrogen inlet and an internal temperature probe was charged with benzhydrylthioacetic acid (3.5 kg, 13.54 mol), methanol (14 L) and H2SO4 (72 g) solution in isopropyl alcohol (6.5 L). To this mixture was added 30% H2O2 solution in water (3.75 L) drop wise over 80 minutes maintaining the temperature below 30 degrees C. Reaction mixture was further stirred for 7 hours, which resulted in formation of a crystalline solid. The reaction was monitored using TLC and HPLC. The resulting solid was filtered and washed with water (4.0 L) to give benzhydrylsulfinylacetic acid (2.5 kg) as a colorless solid. The peroxide was quenched with a NaHSO3 solution.

1. customA 50 L three-necked round bottom flask equipped with a mechanical stirrer
2. temperaturemaintaining the temperature below 30 degrees C
3. customReaction mixture
4. customwhich resulted in formation of a crystalline solid
5. filtrationThe resulting solid was filtered
6. washwashed with water (4.0 L)