2-甲基-5-乙酰氨基苯磺酰氯合成研究

以对甲基苯胺为起始原料,通过乙酰化和氯磺化反应合成2-甲基-5-乙酰氨基苯磺酰氯(Ⅰ)。讨论了乙酰化试剂的选择、反应物料比、反应时间、反应温度等对反应结果的影响。结果表明,以乙酸酐为乙酰化试剂,乙酰化反应温度45~50℃,n(乙酸酐)∶n(对甲基苯胺)=1.2∶1.0,反应进行4 h,氯磺化反应温度50~60℃,n(氯磺酸)∶n(对甲基乙酰苯胺)=4∶1,反应进行8 h,最终目标产物(Ⅰ)收率可达48.5%。

Study on synthesis of 2-methyl-5-acetaminobenzene sulfochloride

Synthesize 2-methyl-5-acetamino benzene sulfochloride using p-toluidine as primer reactant by aceylation and chlorosulfonation.The effects of reaction factors,such as aceylation agent,mole ratio,reaction time and reaction temperature on the reaction was discussed.It was found that the yield of 2-methyl-5-acetamino benzene sulfochloride was up to 48.5% under adefine condition.The condition were as follows:aceylation is 45～50 ℃,n(diacetyloxide) ∶n(p-toluidine)=1.2 ∶1.0,4 h,chlorosulfonation is 50～60 ℃,n(chlorosulfonic acid) ∶n(p-methylacetanilide)=4 ∶1,8 h.