88284-48-4

358-23-6

15288-53-6

88284-48-4

(1) In a 10 L glass reactor, after argon displacement, 6 L of dichloromethane and 1 kg of 2-(trimethylsilyl)phenol (compound III) were added and mixed thoroughly. (2) The reaction system was cooled to -10 to -15 °C using a dry ice-ethanol bath, and 550 g of pyridine was added slowly and dropwise, and the reaction was exothermic and accompanied by the generation of white fumes. (3) Maintain the internal temperature below -10°C and slowly add 1.8 kg of trifluoromethanesulfonic anhydride dropwise. (4) After the dropwise addition, the reaction was carried out at -5 to 0°C for 5 to 6 hours. (5) After confirming the complete consumption of Compound III by GC monitoring, the reaction system was cooled to below 0°C, and the reaction was quenched by slow dropwise addition of 1.5L of 1N hydrochloric acid solution, taking care to control the exotherm. (6) After quenching and stirring, static layering, the organic phase was washed with 2L of saturated sodium bicarbonate solution and 2L of saturated sodium chloride solution, 100g of anhydrous magnesium sulfate drying, filtration and concentration under reduced pressure, to obtain 1.5kg of brown transparent liquid 2-(trimethylmethylsilyl)phenyl trifluoromethanesulfonate (Compound IV). (7) 1.5kg of crude compound IV was transferred to a 2L distillation flask and distilled under reduced pressure. Under 1.0 kPa vacuum, the bath temperature was 91~105°C, boiling point 49~76°C, the pre-fraction F1 (65 g) was collected; the bath temperature was 108~110°C, boiling point 76~79°C, the main fraction F2 (1.32 kg, GC purity 98.7%) was collected; the distillation was stopped and the residue F3 (85 g).