结晶玫瑰制备方法的改进

Improvement of Synthesis of Rosen

通过对结晶玫瑰制备实验的改进,找到了能提高产品产率的最佳实验条件。在第一步反应中,苯甲醛的用量为15mL,氯仿的用量为18mL,加入助溶剂1mL甲醇和20mLDMF,控制在20-30℃之间反应3小时,三氯甲基苯基甲醇的产率为72.90%;在第二步反应中,将14.12g三氯甲基苯基甲醇和8mL乙酸酐反应,加入1mL浓硫酸,在90-110℃之间加热反应3小时,结晶玫瑰的产率最高能够达到85.08%。

In the course of doing experiment, we have explored an optimum method that can boost the yield of the product through a lot of experiments, The first reaction of 15mL benzaldehyde with 18mL chloroform which is composed of 20mL DMF and lmL methanol as solvent should last three hours during 20-30℃. The yield of trichloromethyl-bcnzo-methanol can reach 72.90%. The second reaction of 14.12g trichloromethyl-bcnzo-methanol with 8mL acetic anhydride should last three hours during 90-110℃. The yield ofrosone can reach 85.08%.