合成茴香醛新工艺的研究

Novel synthesis technology of anisaldehyde

以对羟基苯甲醛和碳酸二甲酯为原料,十六烷基三甲基溴化铵为相转移催化剂,在常压下合成茴香醛。考察了溶剂、反应温度、时间和催化剂对反应产率的影响。较佳反应条件为:对羟基苯甲醛10 mmol、碳酸二甲酯100 mmol、十六烷基三甲基溴化铵3 mmol、碳酸钾7 mmol、二甲基亚砜10 mL,130℃反应3 h,产率为88.7%。通过红外光谱和气相色谱质谱联用仪对目标产物进行了表征。

Anisaldehyde was synthesized from p -hydroxybenzaldehyde with dimethyl carbonate under phase transfer catalysts （PTC） hexadeeyhrimethylammonium bromide. Effects of reation temperature and time, as well as solvent and catalyst on yield were investigated. The optimal reaction conditions were found as： p- hydroxybenzaldehyde, 10 mmol; dimethyl carbonate, 100 mmol; hexadecyltrimethylammonium bromide, 3 mmol; potassium carbonate, 7 mmol; dimethyl sulfoxide, 10 mL; reaction temperature 130℃ ; reaction time 3 h. The yield achieves 88.7%. The structure of anisaldehyde was characterized by means of IR and GC - MS.