δ-癸内酯的合成

A NEW METHOD FOR SYNTHESIS OF δ-DECALACTONE

以环戊酮和正戊醛为起始原料,经羟醛缩合、选择性催化加氢、氧化重排制得δ-癸内酯。通过正交实验,得出最佳工艺条件:w(NaOH)=1%,PEG-600用量0.7g,草酸用量0.2g,n(双氧水)∶n(2-戊基环戊酮)=4∶1,甲醇用量30mL,硫酸用量2mL,反应收率为61.2%。采用红外光谱对产物结构进行了表征。

A new method is presented for synthesizing δ-decalactone from n-valeraldehyde and cyclopentanone via the reaction process of aldol condensation,selective catalytic hydrogenation and oxidation.The optimum process conditions acquired through the orthogonal experiments were as follows： w（NaOH） = 1%,m（PEG-600）=0.7 g,m（oxalic acid）=0.2 g,n（hydrogen peroxide）∶n（2-amyl cyclopentanone）=4∶1,V（methanol）=30 mL,V（sulfuric acid）=2 mL,and the final yield was 61.2%,which is superior to the literature reported value of 52%.The intermediates and product were characterized by IR and GC-MS.To compare with the traditional methods,the raw materials are easy available,the reaction route is simple,the product yield is relatively high and the operation is quiet safe via this method.