摘要
以镁粉、2-氯丁烷、正丁基锂为原料合成了两端不同丁基的二丁基镁化合物——正、仲丁基镁。考察了反应温度、反应时间、原料配比等因素对反应的影响,并用1HNMR对合成产物的结构进行了分析。结果表明,反应温度35℃、反应时间4 h、镁粉与2-氯丁烷摩尔比为1.2∶1、乙醚与2-氯丁烷摩尔比为7∶1,格氏试剂的收率达96.1%;反应温度0℃、反应时间0.5 h、格氏试剂与正丁基锂摩尔比为1.0∶1,二丁基镁产率达99%以上。
Dibutylmagnesium, which had two different ends of n-butyl and s-butyl, was synthesized from magnesium powder,2-chlorobutane and n-butyllithium. The effects of reactants ratio, reaction temperature and reaction time on the yield were intensively investigated, and the structure of synthesized product was characterized by ＇HNMR. The experimental results indicated that when the reaction temperature was 35℃, reaction time was 4 h, the molar ratio of magnesium powder to 2-chlorobutane was 1.2： 1 and the molar ratio of ethyl ether to 2-chlorobutane was 7 ： 1, the yield of Grignard reagent reached 96.1%. When the reaction temperature was 0℃, reaction time was 0.5 h and the ratio of Grignard reagent to n-butyllithium was 1.0 ： 1, the yield of dibutylmagnesium was more than 99 %.
出处
《化学与生物工程》
CAS
2009年第7期32-34,共3页
Chemistry & Bioengineering
关键词
二丁基镁
格氏试剂
正丁基锂
2-氯丁烷
正交实验
dibutylmagnesium
Grignard reagent
n-butyllithium
2-chlorobutane
orthogonal experiment
