Gabriel法合成2-(4-氟苯磺酰基)-乙胺

Gabriel-wise synthesis of 2-(4-fluorophenylsulfony) ethylamine

利用Gabriel合成法,以氨基乙醇为起始原料,经取代、氧化、肼解、酸化,得到高纯度的2-(4-氟苯磺酰基)-乙胺盐酸盐,总收率为21.2%,其结构由IR1、H NMR表征确认.考察不同反应条件下对反应收率的影响,确定最优合成工艺条件,氧化反应:115℃,3 h,n(30%H2O2):n(硫醚)=5?1;肼解反应:80℃,5 h,水合肼稍过量.

High-purity 2 - （4 -fluorophenylsulfonyl） ethylamine hydrochloride was obtained with Gabriel synthesis from ethanolammonia as raw material through substitution, oxidation, hydrazine and acidification, with a total yield of 21.2% of the resultant. The structure of the resultant was characterized with IR and 1H NMtL The best reaction conditions were as follows： 115 ℃ ,3 h,n（30% H2O2） ：n（sulfide）= 5 ： 1 for oxidation reaction and 80 ℃,5 h, a little extra hydrazine hydration for hydrazine reaction.