摘要
以硝基甲烷和甲醛为原料 ,在碱性条件下经烷羟基化和溴化两步反应合成了溴硝醇。考察了反应温度、反应时间、溶剂中水与醇的体积比以及溶剂用量对产品收率的影响。最佳反应条件为 :V(水 )∶V(醇 ) =0 4∶1 0 ,V(溶剂 )∶V(反应原料 ) =2 1∶1 0 ,烷羟基化反应时间为 1 5h ,反应温度为 5℃ ;溴化反应时间为 0 5h ,反应温度为 10℃。产品收率可达到 78% ,质量分数为98%。产物经高效液相色谱、红外、质谱确证。
Bronopol was synthesized from nitromethane and formaldehyde by hydroxyalkylation and bromination in the presence of alkali. The effects of reaction temperature, reaction time, the volume ratio of water and alcohol in solvent and the amount of solvent on the yield of the product were investigated. The optimum conditions of the reaction were: volume ratio of water to alcohol 0.4:1.0, volume ratio of solvent to raw materials 2.1:1.0, reaction time of hydroxyalkylation 1.5 h and reaction temperature 5°C, reaction time of bromination 0.5 h and reaction temperature 10°C. The yield of bronopol was 78% with 98% purity. The product was confirmed by HPLC, IR and MS.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2001年第5期257-259,共3页
Fine Chemicals
