新型阳离子光固化活性单体3,3-[氧基双亚甲基]-双[3-甲基]氧杂环丁烷的合成

Synthesis of Bis(3-methyloxetan-3-yl)Methyl Ether for Novel Cationic Photocuringmonomer

在氢氧化钾的作用下,三羟甲基乙烷和碳酸二甲酯通过环化裂解反应生成3-甲基-3-羟甲基氧杂环丁烷;然后在三乙胺的作用下,3-甲基-3-羟甲基氧杂环丁烷与对甲基苯磺酰氯反应,得到3-甲基-3-(对甲基苯磺酸氧基甲基)氧杂环丁烷;在碱性条件下,3-甲基-3-(对甲基苯磺酸氧基甲基)氧杂环丁烷与3-甲基-3-羟甲基氧杂环丁烷醚化得到目标产物3,3-[氧基双亚甲基]-双[3-甲基]氧杂环丁烷。产物经红外光谱和核磁共振谱得到确证。该工艺条件温和,适合工业化生产。

A compound of 3-Methyl-3-hydroxymethyloxetane was firstly prepared by the cyclization cleavagereaction of trimethylolethane and dimethyl carbonate with the catalysis of potassium hydroxide. Then,it reactedwith p-methylbenzene-sulfonyl chloride in the presence of triethylamine to give（3-methyloxetan-3-yl）methyl4-methylbenzenesulfonate. Finally, the（3-methyl-3-（p-toluenesulfonyloxymethyl） oxetane reacted with3-methyl-3-hydroxymethyloxetane in basic conditions to produce the target product of the 3, 3-[oxybismethylene]-bis[3-methyl]oxetan. The products were identified by infrared spectroscopy and nuclearmagnetic resonance spectroscopy. The process conditions are mild and suitable for industrial production.