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以氯代肟基乙酸乙酯和1,1-二苯乙烯在三乙胺催化下经1,3-偶极环加成合成双苯噁唑酸,柱层析分离提纯,产品纯度可达98%以上。中间体氯代肟基乙酸乙酯是以甘氨酸为原料先合成甘氨酸乙酯盐酸盐,再经肟化得到;1,1-二苯乙烯是以溴苯为原料合成格氏试剂苯基溴化镁,和苯乙酮反应生成1,1-二苯乙醇经脱水而得。通过核磁、熔点对中间产物和目标产品进行了结构表征,用高效液相色谱对产品的纯度进行了测定,讨论了中间体和目标产物可能的反应历程及机理。
Chlorinated oxime ethyl acetate and 1,1-stilbene in the triethylamine catalyzed 1,3-dipolar cycloaddition of bis-oxazole acid, column chromatography purification, product purity up to 98 %the above. Intermediates chloroacetic acid ethyl ester glycine as raw materials to the first synthesis of glycine ethyl ester hydrochloride, and obtained by oximation; 1,1-stilbene is brominated benzene as raw materials Grignard reagent phenyl bromide Magnesium, and acetophenone reaction 1,1-diphenyl ethanol obtained by dehydration. The structure of the intermediate and the target product were characterized by NMR and melting point. The purity of the product was determined by high performance liquid chromatography. The possible reaction mechanism and mechanism of the intermediate and the target product were discussed.