preparation | 1) compound 1(1.0g,6.25mmol,1.0eq) and alcl (4.2g,31.50mmol,5.0eq) were added into 30mL cyclohexane at room temperature, the tube was sealed at 110 ℃, and stirred for 2 hours. TLC showed that Compound 1 reacted completely. Add 100mL of ice water to the reaction solution and extract it 3 times with 50mL DCM. The organic phase was washed with 100mL saturated sodium chloride and dried with anhydrous sodium sulfate. The compound 2(0.3g, yield 30%) was obtained by rotating the prep-HPLC under reduced pressure. 2) Compound 2(1.6g,9.9mmol,1.0eq),KCO(5.5g,39.6mmol,4.0eq) and 20mL acetone were added. Seal the pipe and stir at 80 ℃ for 6 hours. TLC showed disappearance of compound 2. The reduced pressure solution of the reaction solution was swirled through the column (PE/EA = 10:1-4:1) to obtain compound 3(0.4g, yield: 25%). |