Gabriel法合成2_4_氟苯磺酰基_乙胺.pdfVIP

35 3 Vol. 35 No . 3 2009 6 Journal of Lanzhou University of Technology Jun. 2009 :2009) Gabriel 法合成2(4氟苯磺酰基)乙胺 苏 策, 贺俊华, 韩丽娟, 张广贵 ( , 730050) : 利用Gabriel 合成法, 以氨基乙醇为起始原料, 经取代氧化 解酸化, 得到高纯度的2( 4氟苯磺酰基)乙 1 胺盐酸盐, 总收率为21. 2% , 其结构由IRH 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% H O ) : n( 硫醚) = 5 1; 解反应: 0 , 5 h, 水合 稍过量. 2 2 : Gabriel 合成法; 2(4氟苯磺酰基)乙胺; 氧化; 解 : O621. 3 : A Gabrielwise synthesis of 2(4fluorophenylsulfony) ethylamine SU Ce, HE Junhua, H AN Lijuan, ZH ANG Guanggui ( College of Petrochem ical T echnology, Lanzhou Univ. of T ech. , Lanzhou 730050, China) Abstract: Highpurity 2 (4 fluorophenylsulfonyl) ethylamine hydrochloride w as obtained w ith Gabriel synthesis from ethanolammonia as raw material through substitution, oxidation, hydrazine and acidifica tion, w ith a total yield of 21. 2% of the resultant. The structure of the resultant w as characterized w ith IR 1 2 2 and H NMR. T he best reaction conditions were as follow s: 115 , 3 h, n( 30% H O ) : n( sulfide) = 5 1 for oxidation reaction and 0 , 5 h, a little extra hydrazine hydration for hydrazine reaction. Key words: Gabriel synthesis; 2(4fluorophenylsulfonyl) ethylamine; oxidation; hydrazinolysis [ 56] 2( 4)( 1, 2 (4 fluorophe ( 6) ; ( 6) nylsulfonyl) ethylamine) ( 1) [ 7] , , ( 1) , ( ) , ( 7) . . 20 50 , Koelzer 1 实验部分 [ 1] , 1. 1 [ 2] M ercury400bb ( ) ; X4 , James ( ) , ( ) ; FTRaman Module [ 3] ( ) . . Gabriel ,