单模聚焦微波催化合成乙酸异戊酯

乙酸异戊酯是一种重要的有机溶剂,在香料、溶剂、萃取剂等方面都有广泛的应用。利用美国CEM公司生产的Discover微波精确有机合成反应器,以冰乙酸、异戊醇为原料,以无水氯化钙和四氯化锡两种无机盐联合作为催化剂合成乙酸异戊酯,并利用傅里叶变换红外光谱仪和折射仪对产品进行了表征。实验中考察了酸醇摩尔比、催化剂用量、微波功率及辐射时间的影响,确定了优化合成条件,实验结果表明,在n(乙酸)/n(异戊醇)为2.5∶1,无水氯化钙-四氯化锡质量为4 g,微波功率为120 W,微波辐射时间为16 min条件下,酯化率可达95.9%。产物乙酸异戊酯经折射仪和红外光谱仪的表征,确定为目标产物。

Synthesis of Isoamyl Acetate Under Signal - Mode Focused Microwave

Isoamyl acetate is an important organic agent,which is extensivly used in spicery,solvent and extractant etc.The discover microwave precision instrument is adopted in this experiment to synthesize isoamyl acetate.Ice acetic acid and isoamyl alcohol is taken as raw material,anhydrous calcium chloride and tin tetrachloride are used as catalyst.The effect of the amount of the catalyst,the power and time of microwave irradiation and the ratio of reactant on the yield was studied.The results show that n(ice acetic)/n(isoamyl alcohol) is 2.5∶1,calcium chloride anhydrous-aluminium chloride is 4 g,irradiation power is 120 W,irradiation time is 16 min,the conversion rate of isoamyl acetate is 95.9%.The results show that the best effect of catalysis is titanium sulfate,which is the best catalyzer of synthesizing isoamyl acetate.The isoamyl acetate was charactered as the target product by IR and refractometer.