摘要
在微波辐射条件下,以草酸、氢氧化钾和溴化苄为原料,四丁基溴化铵为相转移催化剂,聚乙二醇200为溶剂合成了草酸二苄酯,并通过熔点和红外光谱对产物的结构进行了表征。研究了反应物配比、相转移催化剂用量、微波辐射功率、辐射时间等对产物收率的影响。实验结果表明,当n(草酸):n(氢氧化钾):n(溴化苄)=1:2.83:2.34、四丁基溴化铵用量0.15 g、聚乙二醇200用量10 mL、微波功率160 W、辐射时间4.5 min时,草酸二苄酯的收率可达62.96%。
Dibenzyl oxalate was synthesized from oxalic acid, potassium hydroxide and benzyl bromide under microwave irradiation using tetrabutylammonium bromide as phase-transfer catalyst and polyethylene glycol-200 as solvent. Structures of the products were identified by means of melting point measurement and IR. By a single factor test, effects of the reactant ratios, phase-transfer catalyst, microwave power and irradiation time, etc. , on the reaction were studied. Under the optimal reaction conditions, i. e. , n(oxalic acid) : n(potassium hydroxide) : n(benzyl bromide)=1 : 2.83 : 2.34, tetrabutylammonium bromide 0.15 g, polyethylene glycol-200 10 mL, microwave power 160 W and irradiation time 4.5 min, the yield of dimonbenzyl oxalate reached 62.96%.
出处
《精细石油化工》
CAS
CSCD
北大核心
2007年第2期20-22,共3页
Speciality Petrochemicals
基金
陕西省重点实验室科研基金资助项目(05JS38)。
关键词
微波辐射
草酸
氢氧化钾
溴化苄
草酸二苄酯
microwave irradiation
oxalic acid
potassium hydroxide
benzyl bromide
dimonbenzyl oxalate