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首先以三氯化磷、二氯乙酸为原料,N,N-二甲基甲酰胺作催化剂,控制温度85℃,合成了重要反应原料二氯乙酰氯,产率60.8/。然后用氢氧化钠作缚酸剂、三氯甲烷为溶剂,利用二氯乙酰氯、乙醇胺和丁酮为原料,反应温度-4~4℃,搅拌1h,一锅法合成了除草剂安全剂3-二氯乙酰基-2-甲基-2-乙基-1,3-噁唑烷,产率78.6/。最后,对合成的化合物结构应用紫外光谱、红外光谱、核磁共振谱和气相色谱—质谱联机等分析方法进行表征,并对各种光谱谱图进行详细分析。根据光谱数据分析结果确定了除草剂安全剂3-二氯乙酰基-2-甲基-2-乙基-1,3-噁唑烷的结构式。
First, phosphorus trichloride, dichloroacetic acid as raw materials, N, N-dimethylformamide as catalyst, the temperature was controlled at 85 ℃, the synthesis of an important reaction raw material dichloroacetyl chloride, a yield of 60.8 /. Then sodium hydroxide as acid-binding agent, chloroform as solvent, the use of dichloroacetyl chloride, ethanolamine and butanone as raw materials, the reaction temperature -4 ~ 4 ℃, stirring 1h, one-pot synthesis of herbicide safener 3 Dichloroacetyl-2-methyl-2-ethyl-1,3-oxazolidine in a yield of 78.6%. Finally, the structures of the synthesized compounds were characterized by UV, IR, NMR and GC-MS, and the various spectral spectra were analyzed in detail. The structural formula of the herbicide safener 3-dichloroacetyl-2-methyl-2-ethyl-1,3-oxazolidine was determined based on the spectral data analysis results.