2,4-二氯-5-硝基苯基异丙基醚清洁合成工艺研究

Clean Synthesis of 2,4-Dichloro-5-Nitrophenylisopropyl Ether

2,4-二氯-5-硝基苯酚在不同季铵盐催化剂作用下合成2,4-二氯-5-硝基苯基异丙基醚反应研究,发现在二乙基十二烷基苄基溴化铵作用下,2,4-二氯-5-硝基苯酚转化率最高。考察了二乙基十二烷基苄基溴化铵催化剂的用量,反应温度,NaOH加入量以及加入方式对2,4-二氯-5-硝基苯酚转化率的影响。实验结果表明,适宜的工艺条件为催化剂用量1%(mass),95℃,NaOH与2,4-二氯-5-硝基苯酚的物质的量之比为1.5∶1,采用分批加入的方式。在此条件下,合成得到2,4-二氯-5-硝基苯基异丙基醚纯度为94.5%,收率达93%以上。

Synthesis of 2,4-dichloro-5-nitrophenol with isopropylbromine and NaOH over different quaternary ammonium salt as catalyst was studied, and 2,4-dichloro-5-nitrophenol conversion was the highest over diethyltwelvealkylbenzylammoniumbromide. Effects of diethyltwelvealkylbenzylammo- niumbromide dosage, temperature, mole ratio of NaOH to 2,4-dichloro-5-nitrophenol and NaOH feed way were investigated. Experimental results showed that optimal conditions were catalyst dosage 1% （mass）, 95 ℃, mole ratio of NaOH to 2,4-dichloro-5-nitrophenol 1.5 1, batch feed of NaOH, and yield of 2,4-dichloro-5-nitrophenylisopropyl ether over 93 % and purity 94.5 % could be gained.