溴代8-氧杂-螺[4,5]季铵盐的合成

Synthesis of 8-oxa-5-azonia-spiro[4,5]decane bromide

以吗啡啉,1,4-二溴丁烷和无水碳酸钾为原料,以水为溶剂,通过季铵化反应合成出溴代8-氧杂-螺[4,5]季铵盐.研究了原料比、反应温度、回流时间对吗啡啉转化率的影响,结果表明,吗啡啉、1,4-二溴丁烷、无水碳酸钾的用量分别为0.10 mol,0.14 mol和0.11 mol,回流3 h,反应温度为110℃时,吗啡啉转化率达91.7%.最终采用核磁共振、红外光谱、热重分析和液相色谱-质谱联用对产物的结构进行了表征.

Branched 8-oxa-spiro [4,5]quaternary ammonium salt was synthesized by using morpholino,1 ,4-dibromo-butane and anhydrous potassium carbonate as raw materials and using water as solvent through quatern-ization reaction.The effect of material ratio,temperature and reaction time on the conversion rate of morpholino were studied.The results show that:the amount of morpholino,1 ,4-dibromo-butane,potassium carbonate are 0.10 mol,0.14 mol,0.11 mol,refluxed for 3 hours and the temperature is 110 ℃,the conversion rate of mor-pholine was 91.7%.Finally the research characterized the structure of product through HNMR,IR,TG and HPLC-MS.