反应详情

A solution of benzoquinone (23.5 g, 217 mmol) in 500 ml EtOH was added at RT over 30 min to a solution of 4-fluoro-benzenesulfinic acid (34.8 g, 217 mmol) in EtOH (300 mL) and water (500 mL). The resulting solution was stirred 2 h at RT, then diluted to 4 l with warm water. The solution was cooled to 4° C. for 62 h and crystals formed. The crystalline solid was collected by suction filtration and washed with water (3×500 mlL and hexanes (2×500 mL) and dried to give the title compound of Step B (40.8 g). MS (APCI−) Calc.: 268.0, Found: 267.1 (M−1).

1. temperatureThe solution was cooled to 4° C. for 62 h
2. customcrystals formed
3. filtrationThe crystalline solid was collected by suction filtration
4. washwashed with water (3×500 mlL and hexanes (2×500 mL)
5. customdried