摘要
以邻氨基苯甲醚、乙酸酐、氯磺酸、对苯二胺为原料,经乙酰化、氯磺化、酰胺化、脱乙酰基等步骤,研究合成了无致癌性染料中间体N,N'-1,4-苯基二-(3-氨基-4-甲氧基)苯磺酰胺。考察了影响酰胺化反应的因素,其优化条件为:反应物用量n(4-甲氧基-3-乙酰氨基-苯磺酰氯)∶n(对苯二胺)为2.2∶1(摩尔比),反应在40°C进行,反应时间为5.0h。产率可达88.46%。产品经红外、核磁、质谱、元素分析等测定确证了结构。
N,N'-1,4-phenylenebis[3-amino-4-methoxyx-benzenesulfonamide] was synthesized from o-aminoanisole and p-phenylene, diamine and the product was characterized by IR, ~1H NMR and MS. The factors affecting the yield were investigated. The results showed that the optimum conditions are as follows: 4-methoxy-3-acetylamino-benzenesulfonylchloride:p-phenylene diamine, 2.2∶1(mol); reaction temperature,40°C; reaction time, 5.0 h. The yield is above 88.64% under optimum conditions.
出处
《化学世界》
CAS
CSCD
北大核心
2004年第10期534-536,525,共4页
Chemical World
