含双萘环磺酰胺的合成工艺研究  

A Study on the Process for Synthesizing Sulfonamide Containing Two Naphthalene Rings

作　　者：张伟[1] 赵德丰[1] 

机构地区：[1]大连理工大学精细化工国家重点实验室,大连116012

出　　处：《染料与染色》2005年第3期54-56,共3页Dyestuffs and Coloration

基　　金：国家自然科学基金资助项目(20172012)

摘　　要：以7-氨基-4-羟基-2-萘磺酸(J酸、A)为原料,在50-70℃pH=7的条件下,用乙酐酰化得B,然后在乙腈和DMF混合溶液中以碳酸钾为缚酸剂,加入三氯氧磷,在35℃-60℃反应4小时合成了7-氨基-4-羟基-2-萘磺酰氯(C),C用N,N-二甲基乙二胺在乙腈溶剂中回流,在35℃～40℃反应6小时,萃取、重结晶后得标题化合物(D)。与文献报导的工艺相比,省时、工艺稳定、成本降低。用1H,13C-NMR、MS和IR对化合物B、C、D进行了表征。7-Amino-4-hydroxy-2-naphthalenesulfonic acid (J acid, A) was acetylated with acetic anhydride at 50-70℃,pH=7 to give 7-Acetamido-4-hydroxy-2-naphthalenesulfonic acid (B), which was treated with phosphorus oxychloride in a mixture of acetonitrile and DMA at 35-60? for 4 hours, gave 7-Amino-4-hydroxy-2-naphthalenesulfonyl chloride(C). C was condensed with N,N-dimethylethylenediamine in acetonitrile in the presence of postassium carbonate at 35-40℃ for 4 hours, then for 2 hours under refluxing, extracted, recrystalled, gave the title compounds(D). Compared to the literature processes, The process had some advantages of short, stable and low cost. The compounds B, C and D were characterized by 1H,13C-NMR, MS and IR.

关 键 词：双萘环磺酰胺 染料 缩合反应 NMR 

分 类 号：TQ612[化学工程—精细化工]