| 174 | 0 | 103 |
| 下载次数 | 被引频次 | 阅读次数 |
在醋酸溶液中,以间氯苯甲醛、溴酸钾为原料合成间氯苯甲酸,分别研究了反应温度、反应时间、原料配比、溶剂的用量等条件对合成反应的影响,确定了最佳工艺条件.该方法合成间氯苯甲酸的最适宜的操作条件是:反应温度为90℃、反应时间为90 min、n(间氯苯甲醛):n(溴酸钾)=1:0.45,溶剂用量为40 mL(相对于0.1 mol间氯苯甲醛).间氯苯甲酸的收率可达到99.36%以上,间氯苯甲酸产品纯度w(间氯苯甲酸)=99.5%.
Abstract：In the liquor of acetic acid,the catalyzed synthesis of m-chlorobenzoic acid by the reaction of m-chlorobenzal dehyde and potassium bromate was studied.The effects of reaction temperature,reaction time,material ratio,and the amount of catalyst on the synthesis were studied.The proper technological conditions were given as follows:reaction temperature is 90℃;reaction time is 90min;n(m-chlorobenzal dehyde):n(potassium bromate)=1:0.45;the amount of acetic acid solvent is 40mL(based 0.1mol m-chlorobenzal dehyde).The results indicated that the yield rate of m-chlorobenzoic acid can reach 99.36%and purity of the m-chlorobenzoic acid is w(m-chlorobenzoic acid)=99.5%.
[1]张竞,陈声宗,吴灿,等.溴素法-α溴代间氯苯丙酮合成研究[J].化学世界,2003(2):91-93.
[2]胡艾希,陈平,杨郑,等.溴化铜对芳基烷基酮的选择性溴化反应研究[J].中国药物化学杂志,2002,12(6):340-343.
[3]段长强,王兰芬.药物生产工艺及中间体手册[M].北京:化学工业出版社,2002:110.
[4]章思规,辛忠.精细有机化工制备手册[M].北京:科学技术文献出版社,1994:705.
[5]Tmenov D N.Komyush kina T G.Liquid-phase catalytic oxidation of chlorotoluenes[J].Zh.Prild Khim,1977,50(1):133-136.
[6]Samaddar H,Banerice A.Use of potassium bromate:oxida-tion of aldehydes[J].J.Indian Chem.Soc.,1982,59(7):905-906.
[7]Kazuhiko S,Mamoru H,Junko T,et al.Hydrogen peroxide oxidation of aldehydes to carboxylic acid:an organic solvent,halide and metal free procedure[J].Tetrahedron Lett,2000(41):1439-1442.
[8]Anjurn A,Srinivas P.An efficient and mild procedure for preparation of benzoic acids via oxidation of aromatic carbon compounds by employing bromoimides and mercuricacetasystem[J].Chem.Lett.,2001,9(30):900-901.
[9]Linnet P E,Godley A R,Ambrose C A.Micrbial preparation of 3-substituted benzoic acids from 2-substituted phenols GB 2232415[P].1990-12-12.
[10]荆熙瑛,陈式棣,么恩云.红外光谱实用指南[M].天津:天津科学技术出版社,1992:253.
基本信息:
中图分类号:TQ245.12
引用信息:
[1]王树清,高崇,朱石生.由间氯苯甲醛氧化合成间氯苯甲酸的研究[J].南通大学学报(自然科学版),2007,No.21(02):41-43+57.
基金信息:
南通大学自然科学基金项目(03040053)
2007-06-15
2007-06-15