甲酸甲酯与三聚甲醛偶联合成乙醇酸甲酯 Ⅱ.硫酸/金属羰基化合物对收率的影响

Synthesis of methyl glycolate by coupling of methyl formate with trioxane Ⅱ.Effect of sulfuric acid and metal carbonyl

研究了硫酸／金属羰基化合物对甲酸甲酯与三聚甲醛偶联合成乙醇酸甲酯反应的催化作用，结果乙醇酸甲酯和甲氧基乙酸甲酯的收率均有提高；用甲醇分解偶联反应母液，进一步提高了产品收率，优选出较佳的配比，用１０ｍｌ硫酸、３．１２ｇＡｇ２ＳＯ４（Ｉ）所形成的硫酸／金属羰基化合物作催化剂，与４５ｍｌ甲酸甲酯和１２ｇ三聚甲醛进行偶联反应，在甲醇分解偶联反应母液后，得到乙醇酸甲酯和甲氧基乙酸甲酯的摩收率分别为５９．８２％和３４．３９％，超过国外研究结果。

n investigation is carried out on the catalysis of sulfuric acid and metal carbonyl used as a catalyst for the reaction of methyl formate coupled with trioxane. The result shows that both the yields of methyl glycolate and methyl methoxyacetate are improved. Further treatment of the reaction moist with methanol also gives a positive effect. The amount of metal compound is optimized to form metal carbonyl.The yields of methyl glycolate and methyl methoxyacetate are 59.82%(m) and 34.39%(m), respectively, in the reaction of 45 ml methyl formate coupled with 12g trioxane using 10ml sulphuric acid and 0.02mol silver carbonyl as catalyst, which surpasses the result from the foreign patents concerned. Then the reaction moist is decomposed by methanol.