十二水合硫酸铁铵催化合成4-羟基-3-甲氧基肉桂酸戊酯

Synthesis of Amyl 4-Hydroxy-3-Methoxycinnamate Catalyzed by Ammonium Ferric Sulfate Dodecahydrate

以十二水合硫酸铁铵为催化剂,4-羟基-3-甲氧基肉桂酸和正戊醇为原料,直接酯化合成了4-羟基-3-甲氧基肉桂酸戊酯。考察了影响合成反应的主要因素。结果表明,4-羟基-3-甲氧基肉桂酸戊酯的合成优化工艺条件为:4-羟基-3-甲氧基肉桂酸0.2 mol,醇酸摩尔比为2∶1,催化剂用量为6 g,带水剂环己烷30 mL,回流反应3.5 h,在此条件下,收率可达97.0%。通过红外光谱和核磁共振验证了目标产物。催化剂的催化活性高,反应条件温和,方法简便,收率高。

Amyl 4-hydroxy-3-methoxycinnamate was prepared by direct esterification of 3-（ 4-hydroxy-3-me- thoxy-phenyl）-2-propenoic acid and 1-pentanol as raw materials with ammonium ferric sulfate dodecahydrate as a catalyst. The influences of some factors on the synthesis process were studied. The optimal reaction conditions based upon 0. 2 tool of 3-（4-hydroxy-3-methoxyphenyl）-2-propenoic acid were chosen that the molar ratio of 1- pentanol and acid was 2： 1, catalyst 6 g , cyclohexane as watercarrying reagent 30 mL, refluing reaction time 3.5 hours, et al. The yield of the product reaches 97.0 %. The structure of the product is characterized by IR and 1H NMR spectrum. This catalyst is mild, convenient to use, and gives high yields.