抗菌剂溴硝醇的合成

硝基甲烷与25%氢氧化钠溶液同时滴加入甲醛溶液中反应,然后滴加溴反应得到溴硝醇;通过正交实验得出的优化条件为:烷羟基化反应中,n(硝基甲烷)∶n(甲醛)=1∶2.2,反应温度45℃,反应时间1.5 h,n(硝基甲烷)∶n(氢氧化钠)=1∶0.8;溴化反应中,n(硝基甲烷)∶n(溴)=1∶1,反应温度20℃,反应时间1.5 h,在此优化条件下收率达90.5%;产品用红外光谱和高效液相色谱进行分析确认,产品含量为99%。

Synthesis of 2-bromo-2-nitro-1,3-propanediol

In the process for the preparation of 2-bromo-2-nitro-1,3-propaned iol(bronopol),nitromethane is firstly reacted with formaldehyde and alkali metal hydroxide and the reaction m ixture obtained in this way is subsequently reacted with brom ine.Based on orthogonal experiment,the optimum cond itions of the reaction were determ ined.Hydroxyalkylation reaction: the mole ratio of nitromethane to formaldehyde is 1 ∶2.2,reaction temperature is 45℃and time is 1.5 h.The mole ratio of nitromethane to sod ium hydroxide is 1∶0.8.Brom inating reaction: the mole ratio of nitromethane to brom ine is 1∶1,reaction temperature is 20℃and time is 1.5 h.The yield is 90.5% under this cond ition.The product was analyzed and con-firmed by IR spectrum and HPLC,the mass fraction of that is 99%.