N,N'-双氯乙基脲和卡莫司汀的合成研究

N,N'-Mechlorethamine Urea and Carmustine Synthesis

用2-恶唑烷酮、乙醇胺和氯化亚砜制备N,N'-双氯乙基脲,再加入甲酸和亚硝酸钠制得卡莫司汀。分别考察了物料比、反应温度、反应时间等参数,得到N,N'-双氯乙基脲最佳反应条件为:于120℃搅拌加热2h,自然冷却至0℃,加过量氯化亚砜,温度控制在20℃以下。加毕后升温至100℃反应2h。稍降温后加入乙醇和活性炭回流脱色,过滤。在此条件下,N,N'-双氯乙基脲收率达34.4%。

With 2 - oxazolidinone, ethanolamine and thionyl chloride prepared N, N＇- Mechlorethamine urea, and then added with formic acid and sodium nitrite was prepared carmustine. Were investigated the ratio of materials, reaction temperature, reaction time and other parameters, to obtain N, N ＇- Mechlorethamine urea optimum reaction conditions as follows： heated with stirring at 120 ℃ 2h, naturally cooled to 0 ℃, add excess thionyl chloride temperature control in less than 20 ℃. Heated to 100 ℃ plus complete reaction 2h. After cooling slightly, adding ethanol and reflux for decolorization of activated carbon, and filtered. Under this condition, the N, N＇- Mechlorethamine urea yield of 34.4%.