2-(3-硝基亚苄基)乙酰乙酸2-甲氧乙酯的合成

Synthesis of 2-methoxyethyl 2-(3-nitrobenzylidene)acetoacetate

改进了合成 2 - ( 3-硝基亚苄基 )乙酰乙酸 2 -甲氧乙酯的方法。对加料顺序、投料比、反应温度、反应时间等因素对标题化合物收率的影响进行了研究 ,结果表明 ,其最佳条件为先加间硝基苯甲醛和乙酰乙酸 2 -甲氧乙酯 ,后加催化剂浓硫酸 ,间硝基苯甲醛和乙酰乙酸 2 -甲氧乙酯物质的量之比为 1∶ 1 .6,反应时间为 4h,反应温度为 0℃。在上述最佳条件下 ,总收率可达 92 % ,标题化合物的质量分数可达 98%。

The technology of synthesizing 2-methoxyethyl 2-(3-nitrobenzylidene)acetoacetate was improved in this paper. The effect of adding order, ratio of m-nitrobenzaldehyde to 2-methoxyethyl acetoacetate, the condensing temperature and time on the yield of the title compound were also investigated. The result shows that the optimum conditions are as follows: m-nitrobenzaldehyde and 2-methoxyethyl acetoacetate should be added before the catalyst, the ratio of m-nitrobenzaldehyde to 2-methoxyethyl acetoacetate is 1∶1.6, the time is 4 h and the temperature, 0 ℃. Under the optimum conditions the total yield is 92% and the purity of the product is about 98%.