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| 5-羧戊基三苯基溴化膦的合成 | |
| 引用本文： | 杨明庆,张舰,马凌,魏忠林. 5-羧戊基三苯基溴化膦的合成[J]. 精细化工, 2012, 29(4): 391-393 |
| 作者姓名： | 杨明庆 张舰 马凌 魏忠林 |
| 作者单位： | 1. 吉林大学化学学院,吉林长春130012;大庆油田化工有限公司,黑龙江大庆163453 2. 大庆油田化工有限公司,黑龙江大庆,163453 3. 大庆新世纪精细化工有限公司,黑龙江大庆,163511 4. 吉林大学化学学院,吉林长春,130012 |
| 摘 要： | 5-羧戊基三苯基溴化膦广泛用于立体选择性药物的合成。由ε-己内酯和氢溴酸在H2SO4作用下,生成6-溴己酸,再与三苯基膦在甲苯溶剂中缩合生成5-羧戊基三苯基溴化膦(C24H26BrO2P)。通过实验考察了影响5-羧戊基三苯基溴化膦合成的各项因素。结果表明,在n(ε-己内酯)∶n(三苯基膦)∶n(氢溴酸)=1.0∶0.95∶1.4、回流温度反应、反应时间为14 h的条件下,以ε-己内酯计的5-羧戊基三苯基溴化膦收率可达82.2%,经HPLC测定其色谱纯度为98.3%。 |
| 关 键 词： | 5-羧戊基三苯基溴化膦 三苯基膦 ε-己内酯 精细化工中间体 |
| 收稿时间： | 2011-10-24 |
| 修稿时间： | 2011-12-15 |
Synthesis of (5-Carboxypentyl)triphenyphosphonium Bromide |
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| YANG Ming-qing,ZHANG Jian,MA Ling and WEI Zhong-lin. Synthesis of (5-Carboxypentyl)triphenyphosphonium Bromide[J]. Fine Chemicals, 2012, 29(4): 391-393 | |
| Authors: | YANG Ming-qing ZHANG Jian MA Ling WEI Zhong-lin |
| Affiliation: | 1*(1.College of Chemistry,Jilin University,Changchun 130012,Jilin,China;2.Daqing Oilfield Chemical Co.Ltd.,Daqing 163453,Heilongjiang,China;3.Daqing New Century Fine Chemicals Co.Ltd.,Daqing 163511,Heilongjiang,China) |
| Abstract: | The ylid(5-carboxypentyl)triphenyphosphonium bromide is widely used in the synthesis of stereo selectivity drugs.6-Bromohexanoic was synthesized from ε-caprolactone and hydrobromic acid under the action of sulfuric acid,and then was condensed in methylbenzene solvent with triphenylphosphine to produce(5-carboxypentyl)triphenyphosphonium bromide.The effect of reaction conditions on the properties of(5-carboxypentyl)triphenyphosphonium was investigated by method of experiments.The results show that the yield of(5-carboxypentyl)triphenyphosphonium could reach 82.2% and its content was 98.3% calculated by acetylacetone under the following reaction conditions:the molar ratio of ε-caprolactone to triphenylphosphine and hydrobromic acid was 1.0∶0.95∶1.4,and the reaction was effected for 14 h at reflux temperature. |
| Keywords: | (5-carboxypentyl)triphenyphosphonium bromide triphenylphosphine ε-caprolactone fine chemical intermediates |
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