【摘要】 苯甲酰甲酸乙酯是合成除草剂苯嗪草酮的关键中间体。针对苯甲酰甲酸容易在强酸性、高温和强氧化剂条件下脱羰基、脱羟基和氧化分解等问题,采用工业级苯和工业级三氯乙醛为起始原料,合成了较高收率的苯甲酰甲酸乙酯。首先在过量苯与三氯乙醛体系中,用无水三氯化铝催化合成了2,2,2-三氯-1-苯基乙醇;2,2,2-三氯-1-苯基乙醇经过碱解得到2-羟基-2-苯基乙酸;然后将2-羟基-2-苯基乙酸与乙醇酯化,生成2-羟基-2-苯基乙酸乙酯;再通过NaOH-H₂O₂室温氧化2-羟基-2-苯基乙酸乙酯,得到苯甲酰甲酸乙酯。经高效液相色谱法（HPLC）测定,苯甲酰甲酸乙酯的质量分数为98%以上,以三氯乙醛计总收率可达72.12%。更多还原

【Abstract】 Ethyl benzoylformate is a key intermediate for the synthesis of the herbicide of oxazinone.At present,the market gap is large,and domestic demand is basically dependent on imports.In this paper,since that benzoylformic acid is easily decarbonylated,dehydroxylated and oxidatively decomposed under strong acidity,high temperature and strong oxidant conditions,industrial grade of benzene and trichloroacetaldehyde are used as starting materials to synthesize ethyl benzoylformate with a high yield.Firstly,in the excess benzene and trichloroacetaldehyde system,2,2,2-trichloro-1-phenylethanol was synthesized by anhydrous aluminum trichloride,which was alkalized to obtain 2-hydroxy-2-phenylacetic acid.Subsequently,2-hydroxy-2-phenylacetic acid was esterified with ethanol to give ethyl 2-hydroxy-2-phenylacetate.Finally,ethyl 2-hydroxy-2-phenylacetate was oxidized by NaOH-H₂O₂ at room temperature to obtain ethyl benzoylformate.The content of ethyl benzoylformate in the final product was above 98% by high performance liguid chromatography（HPLC）,and the total yield was up to 72.12% based on trichloroacetaldehyde.更多还原