反应详情

27 g of aluminum chloride and 100 ml of toluene were mixed and 25 g of t-butylacetyl chloride was added dropwise to this under ice cooling, After reaction at room temperature for 2 hours, the reaction solution was poured on ice. This was extracted with hexane, and the organic phase was rinsed with water and an aqueous sodium bicarbonate solution, dried and condensed. The crude product was purified by distillation under reduced pressure (95-96° C./2 mmHg) to obtain 32 g of 4-t-butylacetyltoluene. 20 g of 4-t-butylacetyltoluene, 19 g of sodium iodide and 13 g of triethylamine were mixed with 100 ml of acetonitrile, and 13.7 g of chlorotrimethylsilane was gradually added thereto The mixture was reacted at 60° C. for 5 hours, and left alone to be cooled. The reaction solution was poured on ice, this was extracted with diisopropyl ether, and the organic phase was rinsed with an aqueous sodium bicarbonate solution, dried and condensed. This was purified by distillation under reduced pressure (95-98° C./2 mmHg) to obtain 32 g of silylenol ether of 4-t-butylacetyltoluene. Under nitrogen flow, 23.9 g of silylenol ether and 14.8 g of dibutylsulfoxide were dissolved in 100 ml of chloroform. The solution was cooled to −30° C. or less, and to the solution, 19.1 g of trifluoroacetic anhydride was added over 30 min. After reaction at room temperature for one hour, a solution in which 30.8 g of potassium nonafluorobutane sulfonate was dissolved in acetonitrile/water was added to the reaction solution. This was extracted with chloroform, the organic phase was rinsed with distilled water until aqueous phase is neutral. The organic phase was condensed, and the crude product obtained was rinsed with hexane and then with water to precipitate a powder. This was further rinsed with hexane and water by slurry rinsing to obtain 21 g of the compound (I-39).

1. customAfter reaction at room temperature for 2 hours
2. additionthe reaction solution was poured on ice
3. extractionThis was extracted with hexane
4. washthe organic phase was rinsed with water
5. dry with materialan aqueous sodium bicarbonate solution, dried
6. customcondensed
7. distillationThe crude product was purified by distillation under reduced pressure (95-96° C./2 mmHg)