摘要
以2-氨基-4-磺基苯甲酸为原料,经过重氮化、还原,与苯甲醛缩合,生成中间体2-苯亚甲基肼基-4-磺基苯甲酸,再与3-乙酰氨基-5-氨基-4-羟基苯磺酸的重氮盐反应,生成N-(2-羧基-5-磺基苯基)-N'-(5-磺基-2-羟基-3-氨基苯基)-C-苯基甲化合物,经铜离子络合,水解,生成四啮甲1∶1铜络合物.产品经液相色谱分析,纯度98%以上,λmax=603nm,总收率约75%.中间体2-苯亚甲基肼基-4-磺基苯甲酸收率85%以上,结构经1HNMR和MS表征确认.该工艺操作简单,收率较高,已经实现工业化生产.
<Abstrcat> 2-[(phenylmethylene)hydrazino]-4-sulfobenzoic acid was obtained from 2-amino-4-sulfobenzoic acid through diazotization, reduction and condensation with benzaldehyde. This intermediate compound reacted with the diazo salt of 3-acetamino-5-amino-4-hydroxybenzenesulfonic acid, and then through complex with copper ion and hydrolysis to obtain N-(2-carboxyl-5-sulfophenyl)-N'-(5-sulfo-2-hydroxyl-3-aminophenyl)-C-phenylformazan. The HPLC purity of TM is over 98%, λ_(max)=603 nm. The total yield is about 75%. The yield of 2-[(phenylmethylene)hydrazino]-4-sulfobenzoic acid is over 85% and the structure was confirmed by ()~1HNMR and MS. This process in high yield is simple and has been industrializing.
出处
《浙江工业大学学报》
CAS
2005年第3期337-340,共4页
Journal of Zhejiang University of Technology
