2,6-二羟甲基-4-氯苯甲醚(3)和2,6-二羟甲基-4-苯基苯甲醇(4)与三缩四乙二醇和四缩五乙二醇的二对甲苯磺酸酯在含有叔丁醇钾的无水四氢呋喃中反应生成甲氧基冠醚5—7。后者与过量无水碘化锂在无水吡啶中廻流有选择性地除去甲基而不影响大环苄醚基的破裂生成三种2’-羟基-1’,3’-亚苯基二甲基冠醚8—10,产率为85—89％。 2,6-dimethylol-4-chloroanisole (3) and 2,6-dimethylol-4-phenylbenzyl alcohol (4) with tetraglycol and tetrapentaethylene glycol Of bis-tosylate in anhydrous tetrahydrofuran containing potassium tert-butoxide to form methoxy crown ether 5-7. The latter with an excess of anhydrous lithium iodide in anhydrous pyridine bleed selectively remove the methyl group without affecting the macrocyclic benzyl ether rupture to generate three 2’-hydroxy-1 ’, 3’-phenylene Dimethyl crown ether 8-10, the yield was 85-89%.