摘要
研究了在不同的溶剂和后处理方式下３种３－硝基－Ｎ－乙基咔唑的单溴化方法：（１）冰醋酸－水稀释法；（２）冰醋酸一蒸馏法；（３）１，２－二氯乙烷一蒸馏法。比较了３种方法各自的优缺点，认为（３）法是较佳的工业化路线。按此工艺路线，在最佳工艺条件即３．硝基．Ｎ－乙基咔唑与溴的摩尔比为１：１、反应时间为３ｈ反应温度为１５℃、溶剂的量为２．５ｍｌ／ｍｍｏｌ下，收率达到９６．０％。
Three monobromination methods of 3 - nitro N- ethylcarbazole were studied according to solvent used and separation process. Method l: acetic acid - diluted with water; 2: acetic acid - decantation; 3: 1, 2-dichloroethane- decantation. The advantages and disadvantages of the three methods were discussed. It was considered that method 3 is the best route in the future industrial production. Under the optimum conditions, those are foe molar ratio of materials is 1:1, the reaction the is 3h,the reaction remperature is 15t,the amount of solvent is 2.5ml/mmol, the yield is 96.0%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
1999年第2期47-49,共3页
Fine Chemicals
关键词
硝基
乙基咔唑
溴化
工艺
合成
染料
中间体
3-nitro N-ethylcarbazole
monobromination
technology
synthesis
