高纯度3-硝基-4-氯苯磺酰氯的制备

SYNTHESIS OF 4-CHLORO-3-NITROBENZENE SULFONYL CHLORIDE WITH HIGHER PURITY

以邻硝基氯苯和氯磺酸为原料合成3-硝基-4-氯苯磺酰氯,考察了反应温度、反应时间和反应物投料摩尔比对产物收率的影响,并用非极性溶剂或弱极性溶剂进行重结晶.结果表明:反应温度120℃,反应时间4h,n(氯磺酸):n(邻硝基氯苯)=4:1,最终用石油醚对粗产物进行重结晶,收率达81.5%,纯度达99.96%(质量分数),经IR、1H NMR分析确定为3-硝基-4-氯苯磺酰氯.

4-Chloro-3-nitro-benzene sulfonyl chloride was prepared from chloro-sulphonic acid and o-chloro-nitro-benzene.The effects of reaction temperature,time and stuff molar ratio on the yield were studied.The product was recrystallized by non-polar or low-polar solvent.The results showed that the optimal reaction temperature is 120‰,reaction time is 4 h,molar ratio of chloro-sulphonic acid to o-chloro-nitro-benzene is 4:1,and then the raw product was recrystalized by petroleum ether. Under these conditions,the product yield is 81.5% and its purity is 99.96%.The product was char- acterized by ~1H NMR and IR.