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在微波辐射条件下,以3,4-二羟基苯甲醛和乙酰甘氨酸为原料,经Knoevenagel缩合,水解后得到α-乙酰氨基-β-(34,-二乙酰氧基苯基)丙烯酸,再用盐酸水解制得β-(3,4-二羟基苯基)丙酮酸,经Clemmensen还原制得标题化合物,总收率36.7%。以反应温度、反应时间、微波辐射功率为影响因素进行正交试验。在前两步反应中,辐射功率是影响反应的主要因素。与传统方法相比,前两步反应使用微波条件,反应产率分别为90.8%和88.6%,并且反应时间大为缩短,分别为15和8 min。
Under microwave irradiation, 3,4-dihydroxybenzaldehyde and acetylglycine as raw materials, after Knoevenagel condensation, hydrolyzed to give α -acetylamino - β - (34, - diacetoxyphenyl) acrylic acid, Hydrochloric acid hydrolysis of β- (3,4-dihydroxyphenyl) pyruvate, Clemmensen reduction of the title compound, the total yield of 36.7%. The orthogonal experiment was carried out with reaction temperature, reaction time and microwave radiation power as influencing factors. In the first two reactions, the radiation power is the main factor affecting the reaction. Compared with the traditional method, the first two reactions using microwave conditions, the reaction yield was 90.8% and 88.6%, and the reaction time was greatly reduced, respectively, 15 and 8 min.