托莫西汀合成中间体3-甲氨基-1-苯丙醇的合成研究

The Synthesis Investigation for 3-Methylamino-1-Benzyl Alcohol

论文研究了3-甲氨基-1-苯丙醇（MPP）的制备方法。文中以苯乙酮为原料,经曼尼希反应,而后使用硼氢化钾还原,制得MPP,并对反应条件进行了探索,研究发现3-甲胺基-1-苯基-1-丙酮盐酸盐的最佳制备条件为p H 3~4,78.5℃,反应6 h,最大产率62.84%;MPP最佳合成温度为3℃,处理时甲苯为萃取剂,正己烷为重结晶溶剂,收率为72.02%,纯度达到88.35%。在以上反应条件下,产物总收率为45.25%。

The synthesis method for 3-methylamino-1-benzyl alcohol was investigated. The 3-methylamino-1-benzyl alcohol was synthesized with acetyl benzene as start material, through mannich reaction, and then reduced with KBH4. The best reaction condition for compound 3-methylamino-1-phenyl-1-acetone hydrochloride was at pH 3~4 , reacted 6 h under 78. 5℃ with 62. 8% yield. The best reaction condition for compound 3-methylamino-1-benzyl alcohol was 3 ℃, with toluene as extracting agent, n-hexane as recrystallization solvent, with 72. 0% yield and 88. 4% purity. Under upper reaction condition, the total yield for final product was 45. 3%.