摘要
在缚酸剂存在下,以乙二醇为羟乙基化试剂对2,4-二硝基氯苯(DNCB)进行羟乙基化合成了β-(2,4-二硝基苯氧基)乙醇(2,4-DNPE),并用元素分析、IR和1H NMR进行了结构表征。考察了缚酸剂类型及其用量、反应温度和时间、乙二醇与DNCB的物质的量的比对反应的影响。结果表明:NaOH是较为适宜的缚酸剂;在n(NaOH):n(DNCB)=1.25:1.0、n(乙二醇);n(DNCB)=6.0:1.0、反应温度65℃和反应时间6 h条件下,2,4-DNPE收率约95%。
In the presence of acid-binding agents, 2,4-dinitrochlorobenzene (DNCB) was hydroxyethylated with ethylene glycol (EG) as hydroxyethylating agent. The product 2,4-Dinitrophenoxyethanol (2,4-DNPE) was confirmed by elemental analysis, IR and ^1H NMR. HPLC analysis showed that the content of 2,4-DNPE in the product was above 99%. The influences of the types and amounts of acid- binding agents, reaction temperature, reaction time and the mass ratio of EG to DNCB in the reaction were investigated. The experimental results showed that NaOH was a very suitable acid-binding agent. When n(NaOH) : n(DNCB)1. 25 : 1.0, n(EG) : n(DNCB)= 6.0 : 1.0, reaction temperature 65 ℃ and reaction time 6.0 h,the yield of 2,4-DNPE based on DNCB was about 95%.
出处
《精细石油化工》
CAS
CSCD
北大核心
2007年第2期23-26,共4页
Speciality Petrochemicals
基金
盐域工学院应用化学重点学科建设基金资助(XKY2006028)。