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我们采用质子性溶剂(甲基溶纤素、乙基溶纤素、异戊醇、正戊醇)对苯并类冠醚的合成方法进行了改进,使反应时间大大缩短.例如,在上述质子性溶剂中反应2—4小时,能使二苯并-18-冠-6、苯并-15-冠-5的产率达到或者接近Pedersen的产率.此外,在合成苯并-15-冠-5时,我们还采用二甲亚砜、正丁醇、二(口恶)烷、四氢呋喃作溶剂进行了一些条件试验,结果表明:采用改进了的Williamson法合成苯并类冠醚,反应必须在90℃以上才能进行。用质子性溶剂(醇类、醇类—水)可以促进反应进行,采用质子性溶剂时,提高反应温度能加快反应速度.
We have used protonated solvents (methyl cellosolve, ethyl cellosolve, isoamyl alcohol, n-amyl alcohol) to improve the synthesis of benzo crown ethers and greatly shorten the reaction time.For example, in the proton Solvent for 2-4 hours, the yield of dibenzo-18-crown-6 and benzo-15-crown-5 can reach or close to that of Pedersen.In addition, in the synthesis of benzo-15-crown -5, we also carried out some conditions tests using dimethyl sulfoxide, n-butanol, dioxane and tetrahydrofuran as solvents. The results show that the modified Williamson method can synthesize benzo crown ethers. Above 90 ℃ can be carried out. With protic solvents (alcohols, alcohols - water) can promote the reaction, the use of protic solvents, increasing the reaction temperature can speed up the reaction rate.