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微波辐射活性炭负载磷钨酸催化合成季戊四醇双缩酮(醛)
引用本文:袁先友,蒋小平,张敏,尹笃林.微波辐射活性炭负载磷钨酸催化合成季戊四醇双缩酮(醛)[J].合成化学,2003,11(1):52-55,64.
作者姓名:袁先友  蒋小平  张敏  尹笃林
作者单位:1. 零陵学院化学系,湖南,永州,425006
2. 湖南师范大学化学化工学院,湖南,长沙,410081
基金项目:湖南省教育厅重点资助项目 ( 0 2 B0 2 5 )
摘    要:在微波辐射下,以活性炭负载磷钨酸为催化剂,不用溶剂,合成了8种季戊四醇双缩酮(醛),以环己酮与季戊四缩的缩合为模型反应进行优化,其优化反应条件为:季戊四醇2.0g,催化剂0.3g,环己酮4.0mL,微波输出功率600W,辐射时间3min,产率达95.4%,该条件下的反应速度是常规加热反应速度的30倍,所得产物经元素分析,IR和1H NMR表征。

关 键 词:季戊四醇双缩酮  微波辐射  活性炭负载磷钨酸  季戊四醇  缩醛  合成  催化剂
文章编号:1005-1511(2003)01-052-04

Synthesis of Diacetals and Diketals of Pentaerythritol under Microwave Irradiation Catalyzed by HPW/C
YUAN Xian-you ,JIANG Xiao-ping ,ZHANG Min ,YIN Du-lin.Synthesis of Diacetals and Diketals of Pentaerythritol under Microwave Irradiation Catalyzed by HPW/C[J].Chinese Journal of Synthetic Chemistry,2003,11(1):52-55,64.
Authors:YUAN Xian-you  JIANG Xiao-ping  ZHANG Min  YIN Du-lin
Institution:YUAN Xian-you 1,JIANG Xiao-ping 1,ZHANG Min 1,YIN Du-lin 2
Abstract:Diketals and diacetals were synthesized from 2,2-bis(hydroxymethyl)propane-1,3-diol with aldehydes and ketones under microwave irradiation using phosphotungstic acid supported on active carbon as a catalyst. Under the optimum reaction conditions(pentaerythritol 2.0g, HPW/C 0.3g, cyclohexanone 4.0mL, microwave power 600W, microwave irradiation time 3min),the yield of diketal was 95.4%. The reaction was 30 times faster under microwave irradiation than conventional heating. The products were characterized by elemental analysis, IR and 1H NMR.
Keywords:microwave irradiation  phosphotungstic acid supported on active carbon  2  2-bis(hydroxymethyl)propane-1  3-diol  diketalization  diacetalization  synthesis  
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