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先经三步反应制得产物[3],其红外光谱与文献值相符。在装有搅拌器,回流冷凝器的三口瓶中,放入干燥过的苯和吡啶,加入[3],再滴加SOCl_2与苯的混合液,回流搅拌八小时,放置过夜,过滤,苯洗,减压除去残留溶剂,得产物[4],为桔红色固体,产率85％。在装有搅拌器、带干燥管的冷凝器及滴液漏斗的三角瓶中,放入PMBP,加入二氧六环,在水浴上加热溶解,在80℃下加入Ca(OH)_2细粉。再在强烈搅拌下滴加产物[4]与二氧六
The first three-step reaction products [3], the infrared spectra consistent with the literature. In a three-necked flask equipped with a stirrer and a reflux condenser, dried benzene and pyridine were placed and added [3], and then a mixed liquid of SOCl_2 and benzene was dropwise added. The mixture was stirred under reflux for eight hours, left overnight, filtered, , The residual solvent was removed under reduced pressure to give the product [4] as an orange solid with a yield of 85%. A flask equipped with a stirrer, a condenser with a drying tube, and a dropping funnel was charged with PMBP, dioxane was added, the mixture was heated and dissolved in a water bath, and fine powder of Ca (OH) 2 was added at 80C. The product [4] and dioxane were then added dropwise with vigorous stirring