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3 Example 3: Preparation of Compound 1
Take 44 g of compound 8, add it to 760 g of methanol, cool it to 0-5 °C, add 135.6 g of thionyl chloride dropwise, stir for 30 min, heat up to reflux, keep the temperature for 24 h, cool down to room temperature after the reaction, pour it into 1000 g Quenched in 5% sodium bicarbonate solution, a large amount of solid was precipitated, stirred for 30 min, filtered, and the filter cake was washed with water and dried to obtain a crude product of compound 1, which was then recrystallized with DMF to obtain 44.9 g of compound 1 with a yield of 95.2%.
1-7 Example 1:
Take 120g of compound 2, dissolve it in 600g of diphenyl ether, mix it into a homogeneous phase, and pump it into a tubular reactor (inner diameter 4mm, length 2m) with a constant-flow pump, the reactor temperature is 255 ° C, and the reaction residence time is 4min , the outlet liquid was collected, and the conversion rate was 88.3% detected by HPLC. After the liquid was cooled to separate out the solid, 600 g of petroleum ether was added to stir and disperse, and the crude product was filtered to obtain 90.7 g of the product with a yield of 82.2%.