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三光气替代制备5-硝基-2-氯苯磺酰氯


全文字数:7000字左右  原创时间:<=2022年

【内容摘要】

三光气替代制备5-硝基-2-氯苯磺酰氯


三光气替代制备5-硝基-2-氯苯磺酰氯
摘要:本文以5-硝基-2-氯苯邻磺酸为原料通过三光气(BTC)替代合成重要染料中间体5-硝基-2-氯苯磺酰氯,通过IR、NMR表征产物。并对反应温度、投料比、反应时间等工艺进行研究,表明最佳的工艺条件是50 ℃下,反应物的摩尔比n(5-硝基-2-氯苯磺酸):n(三光气)= 4:1,四氢呋喃作为溶剂,反应时间4 h,收率为88.3 %。

关键词:5-硝基-2-氯苯磺酸,5-硝基-2-氯苯磺酰氯,BTC
Synthesis of 5-Nitro-2-Chlorobenzenesulfonyl Chloride
by Triphosgene
 
Abstract: The important dye intermediate of 5-nitro-2-chlorobenzenesulfonyl chloride had been gotten from 5-nitro-2-chloro-benzenesulfonic acid using Bis(trichloromethyl)carbonate (BTC) . The products were characterized by IR, NMR. And the reaction temperature, catalyst amount, reaction time, solvent were also investigated. The optimum reaction condition was the mole ratio of 5-nitro-2-chloro-benzenesulfonic acid: BTC = 4:1, tetrahydrofuran as solvent, reaction time 4 h, reaction temperature 50 ℃. Under this optimum reaction, the yield of 88.3 % could be got.

Key Words: 5-nitro-2-chlorobenzenesulfonic acid, 5-nitro-2-chlorobenzenesulfonyl chloride, Bis(trichloromethyl)carbonate (BTC)

 

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