α-甲氧甲酰基-γ-丁内酯和α-乙氧甲酰基-γ-丁内酯的合成及表征

Synthesis and characterization of α-methoxyformyl-γ-butyrolactone and α-carbethoxy-γ-butyrolactone

以γ-丁内酯为原料,分别与碳酸二甲酯、碳酸二乙酯,在氢化钠的催化下,利用α氢的活泼性制得α-甲氧甲酰基-γ-丁内酯和α-乙氧甲酰基-γ-丁内酯。探索了反应温度、反应时间、反应物配比、催化剂用量对产率的影响。结果表明,适宜的反应条件为:①合成α-甲氧甲酰基-γ-丁内酯反应温度25℃,催化剂0.3 mol,反应时间3 h,反应物料物质的量比1∶1.5,产率可达85%;②合成α-乙氧甲酰基-γ-丁内酯反应温度30℃,催化剂0.3 mol,反应时间4 h,反应物物质的量比1∶2,产率可达76%。对产品进行了核磁共振氢谱、红外光谱表征。

α-Methoxyformyl-γ-butyrolactone and α-carbethoxy-γ-butyrolactone were synthesized usingγ-butyrolactone as raw material with dimethyl carbonate and diethyl carbonate by the chemical activity ofα-hydrogen under sodium hydride respectively. The influence of reaction temperature,reaction time,react-ant ratio and catalyst dosage on product yield were studied. The result showed that the optimum reaction conditions were as follows：α-methoxyformyl-γ-butyrolactone：reaction temperature 25 ℃,reaction time 3 h,n（γ-butyrolactone）： n（dimethyl carbonate）= 1 ： 1. 5,the amount of catalyst was 0. 3 mol,the yield of the product was ≥85% ;α-carbethoxy-γ-butyrolactone：reaction temperature 30 ℃,reaction time 4 h, n（γ-butyrolactone）： n（diethyl carbonate）= 1 ： 2,the amount of catalyst was 0. 3 mol,the yield of the product was ≥76% . The products were characterized by 1 H NMR and FTIR.