摘要
在四氢呋喃/水混合相溶剂中,以锌粉参与的经典烯丙基化反应合成了标题化合物,利用核磁(1HNMR)、红外光谱和质谱(LRMS)表征了其结构,利用气相色谱仪测试了其纯度,并讨论了甲代烯丙基溴与锌粉的物质的量比、反应时间及温度等影响因素,确定了该反应的最佳条件;同时,在甲苯/水混合相溶剂中和少量醋酸作用下,以甲代烯丙基氯为起始原料合成了标题化合物,原料易得,操作方便,具有应用于工业化生产的潜力。
The classic allylation reaction mediated by zinc powder to synthesis of 3-methyl-3-butene-l-ol （MBOH） in tetrahydrofuran/water. The structure was confirmed by the nu- clear magnetic resonance （IH and 13CNMR）,IR and mass spectrometry （LRMS）. The purity was checked by GC up to 99%. The optimization of conditions to synthesis 3-methyl-3- butene-l-ol was discussed by the molar ratio of reagents, the time, the temperature and other factors. Meanwhile, the syn- thesis of 3-methyl-3-butene-1 -ol from methallyl chloride under a small amount of acetic acid in toluene/water solvent was al- so readily available. The operation was convenient, and it is potential to further applied in industrial production.
出处
《化学试剂》
CAS
CSCD
北大核心
2013年第10期944-946,共3页
Chemical Reagents
基金
国家自然科学青年基金资助项目(51208236)
江苏省自然科学青年基金资助项目(BK20131011)
