摘要
以间氨基苯磺酸为原料 ,经乙酰化保护氨基 ,用氯磺酸 /氯化亚砜将磺酸基转变为磺酰氯 ,再分别与氨基G酸、吐氏酸、布龙酸、γ-酸、6-氨基 -1 ,3-萘二磺酸、5 ,6-二氨基 -1 ,3-萘二磺酸胺化缩合 ,水解去乙酰基 ,较高收率地合成了间氨基 -N -取代 -苯磺酰胺类染料中间体。产物结构经元素分析、红外。
Dye intermediates m amino N alkylsubstituted benzenesulfonamide have been synthesized from m amino benzenesulfonic acid in high yield through the acetylation of amido, chlorination of the sulfonic group, amidation and hydrolysis. SOCl 2/ClSO 3H was used as the reagent of chlorination at 50℃~60℃ with the molar ratio of m acetylamino benzenesulfonic acid Na salt∶ClSO 3H∶SOCl 2 = 1∶5∶3. m Acetamido benzenesulfonyl chloride was dissolved in acetic ether before amidation at 50℃~60℃ in 2h with amino G acid, Tobia acid, Brooner's acid, γ acid, 6 amino 1,3 naphthalenedisulphonic acid and 5,6 diamino 1,3 naphthalenedisulphonic acid, respectively. The pH value of the amidation reaction solution was controlled at 7~8 with sodium carbonate solution. The products were characterized by EA, IR, 1H NMR and MS.
出处
《合成化学》
CAS
CSCD
2002年第1期62-64,共3页
Chinese Journal of Synthetic Chemistry