O-甲基异脲硫酸氢盐的合成

Synthesis of O-Methyl-isoure Hydrogen Sulphate

采用浓硫酸和甲醇预混液滴加到单氰胺与甲醇混合液的方法合成了O-甲基异脲硫酸氢盐。考察了物料配比、反应时间、反应温度、浓硫酸滴加方式及洗涤溶液的种类对产品收率和纯度的影响。得到较佳的工艺条件为:n(单氰胺)∶n(硫酸)∶n(甲醇)=1∶1.5∶5,反应温度5℃,反应时间3h,丙酮洗涤。产品收率可达74.4%,产品纯度可达98.1%。产品用FT-IR进行了表征。

O-methyl-isoure hydrogen sulphate was synthesized using cyanogenamide,methanol and sulfuric acid as starting materials.The effect of n（cyenogenamide）：n（sulfuric acid）：n（methanol）,reaction time,reaction temperature,the addition method of sulfuric acid and washing agents on the yield and purity of product were investigated.The obtained optimum reaction conditions were n（cyanogenamide）∶n（sulfuric acid）∶n（methanol） =1∶1.5∶5,reaction temperature 5 ℃,reaction time 3 h and using acetone as washing agent.Under above conditions,the yield and purity of product were 74.4% and 98.1% respectively.The structure of the obtained product was characterized by FT-IR.