3-溴甲基-3-甲基氧杂环丁烷的合成

Synthesis of 3-Bromonomethyl-3-Methyloxetane

以2,2-二溴甲基丙醇(BBMP)为初始原料,通过与碱发生关环反应生成3-溴甲基-3-甲基氧杂环丁烷(BrMMO)。讨论了碱的种类和用量对BBMP关环产率的影响以及反应体系中碱的浓度、反应温度和反应时间对合成BrMMO产率的影响。通过实验确定的最佳工艺条件为:BBMP与NaOH摩尔比为1.0∶1.1,NaOH醇溶液的质量分数为12%,反应温度为78℃,反应时间为4h时,BrMMO产率为65%。最终产品经元素分析、IR和1HNMR检测确定为BrMMO。该试验工艺简单,原料易得,且溶剂便于回收、污染小。

The 3-bromomethyl-3-methyloxetane （BrMMO） was synthesized by the dosed-ring reaction between 2, 2-dibromomethyl propanol （BBMP） as primary substance and alkaIi. The effect of kinds of alkali and its amount on the closed ring yield of BBMP was discussed. The effect of the base concentration, reaction temperature and the reaction time on the yield of BrMMO in the closed-ring reaction was discussed. Under the reaction conditions of n（BBMP） ： n（NaOH）=l. 0 ： 1. 1, NaOH mass fraction 12%, reaction temperature 78℃, reaction time 4h, the yield of BrMMO was 65%. The structure of BrMMO was identified by elemental analysis,IR and IHNMR. The results showed that it was the target compound BrMMO. This experiment process was easy to do, raw material was liable to attain, and the solvent can be retrieved, so the pollution was small.