一锅法合成螺环二醇

Synthesis of Spiroglycol by One-pot Method

采用一锅法对螺环二醇的合成进行了研究。较佳反应条件为:第一步反应中,甲醛、异丁醛、三乙胺的用量分别是2.9,2.7,0.07mol,反应时间6h,反应温度70℃;第二步反应中,季戊四醇和盐酸的用量分别是1.0mol和0.06mol,反应时间10h,反应温度60℃。在此条件下,螺环二醇的总收率为93.6%,含量大于99.0%。探讨了该合成过程的反应机理。采用IR和1HNMR对产物结构进行了表征。

A novel method of synthesis of spiroglycol by one - pot reaction was studied. The optimum reaction conditions were ： in the first stage, amount of formaldehyde, isobutyl aldehyde, and triethylamine respectively 2.9,2.7, and 0.07 mol, reaction time 6 h, reaction temperature 70 ℃ ; in the second stage, amount of pentaerythritol and hydrochloric acid respectively 1.0 and 0.06 mol ,reaction time 10 h, reaction time 60 ℃. Under above conditions, the total yield and purity of spiroglycol were 93.6 % and 99.0 % respectively. The reaction mechanism of the synthetical process was discussed. The product was characterized by ^1H NMR and IR.