喹啉臭氧化-脱羧合成烟酸
Preparing nicotinic acid by ozonolysis-decarboxylation of quinolineb
查看参考文献20篇
|
文摘
|
报道了在常压和低温下,在冰乙酸、乙酸乙酯和水的混合溶剂中臭氧化喹啉得到2,3-吡啶二羧酸,然后升华脱羧制备烟酸.试验考察了浓硫酸和溶剂对烟酸产率的影响,最佳反应条件为:n(浓硫酸)∶n(喹啉)=(1.1～1.5)∶1;V(冰乙酸)∶V(乙酸乙酯) = 3∶1.在该条件下2,3-吡啶二羧酸收率可稳定在66%以上,脱羧后得到烟酸,产率高于96%,熔点235～237.3 ℃,HPLC测得相对质量分数在95%以上. |
|
其他语种文摘
|
Nicotinic acid is an important intermediate for pharmaceuticals and fine chemicals,and it is estimated that the domestic demand will exceed 5000 tons by 2010.In this paper,nicotinic acid was prepared by subliming amd decarboxylation of pyridine-2,3-dicarboxylic acid(quinolinic acid) which was obtained from the ozonolysis of quinoline in a solvent containing glacial acetic acid,acetic ether and water under mild reaction.Through the experiment,the influences of concentrated sulfuric acid and solvents on the yield of nicotinic acid were investigated.The optimum molar ratio of n(concentrated sulfuric acid)︰n(quinoline)=(1.1～1.5)︰1;V(glacial acetic acid)︰V(acetic ether) = 3︰1.Under the above conditions the yield of pyridine-2,3-dicarboxylic acid was up to 66%.Nicotinic acid was obtained by decarboxylation of pyridine-2,3-dicarboxylic acid with a yield of more than 96% and the melt point was 235～237.3℃.The relative mass fraction was no less than 95% detected by HPLC.
|
|
来源
|
化工进展
,2007,26(8):1125-1128 【核心库】
|
|
关键词
|
烟酸
;
臭氧化
;
2,3-吡啶二羧酸
;
喹啉
|
|
地址
|
中国科学院新疆理化技术研究所, 新疆, 乌鲁木齐
|
|
语种
|
中文 |
|
文献类型
|
研究性论文 |
|
ISSN
|
1000-6613 |
|
学科
|
生物化学;生物物理学 |
|
文献收藏号
|
CSCD:2910306
|
参考文献 共
20
共1页
|
|
1.
Hoelderich W F. 'One-pot'reactions:a contribution to environmental protection applied.
Catalysis A:General,2000,194/195:487-496
|
被引
1
次
|
|
|
|
|
2.
Jar(a)s S. Preparation of pyridinemonocarboxylic acids by catalytic vapor phase oxidation of alkylpyridine.
J Appl Chem Biotechnol,1977,27(3):499
|
被引
1
次
|
|
|
|
|
3.
Heinz D.
Process for the preparation of nicotinic acid US,6 229018BI,2001
|
被引
1
次
|
|
|
|
|
4.
殷洪.
烟酸制造新工艺 中国,1141288,1997
|
被引
1
次
|
|
|
|
|
5.
Woodward C F. Chemical-catalytic liquid-phase oxidation of nicotine 3-picoline and quinoline to nicotinic acid.
Industrial And Engineering Chemistry,1944,36(6):544-546
|
被引
1
次
|
|
|
|
|
6.
Suga S.
Method of measuring and controlling ozone concentration US 4983526,1991
|
被引
1
次
|
|
|
|
|
7.
Azuma K.
Apparatus for measuring ozone concentration US 4849178,1989
|
被引
1
次
|
|
|
|
|
8.
Bailey P S.
Ozonation in Organic Chemistry,1982
|
被引
3
次
|
|
|
|
|
9.
Tamar M. Reactive uptake of ozone by aerosol-associated unsaturated fatty acids:kinetics mechanism and products.
J Phys Chem A,2002,106(27):6469-6476
|
被引
2
次
|
|
|
|
|
10.
沙耀武. 臭氧化物生成机理研究综述.
有机化学,1999,19(3):224-235
|
被引
8
次
|
|
|
|
|
11.
Willard R W. The electronic structure of the criegee intermediate ramifications for the mechanism of ozonolysis.
J Am Chem Soc,1975,97(11):3004-3021
|
被引
1
次
|
|
|
|
|
12.
Sun Z C. Oxidation of glyoxal with hydroperoxide compounds prepared from maleic acid by ozonation to produce glyoxylic acid.
Ind Eng Chem Res,2006,45(6):1849-1852
|
被引
2
次
|
|
|
|
|
13.
Benbelkacem H. The oxidation of some azaarenes with ozone.
Ozone:Science and Engineering,2002,24(3):271-280
|
被引
1
次
|
|
|
|
|
14.
Shive W. Ozonolysis of pyridine homologs a method of structural elucidation.
J Am Chem Soc,1946,68(11):2144-2148
|
被引
1
次
|
|
|
|
|
15.
Emil J M. Heteropolar ozonization of aza-aromatics and their N-oxides.
J Am Chem Soc,1964,86(1):38-46
|
被引
1
次
|
|
|
|
|
16.
Del R E. Solvent effects on ozonolysis reaction intermediates.
Chemical Physics Letters,1997,280(5):444-450
|
被引
1
次
|
|
|
|
|
17.
Nawrocki J. Influence of ozonation conditions on aldehyde and carboxylic acid formation.
Ozone:Science and Engineering,2003,25(1):53-62
|
被引
6
次
|
|
|
|
|
18.
William H B. Preparation properties and reactions of carbonyl oxides.
Chem Rev,1991,91(3):335-362
|
被引
1
次
|
|
|
|
|
19.
Russeljl M. Decarboxylation of 5-substituted 2-pyridinecarboxylic acids.
J Org Chem,1972,37(24):3938-3940
|
被引
1
次
|
|
|
|
|
20.
Cantwell N H. Effect of methyl substitution on the decarboxylation of picolinic acids.
J Am Chem Soc,1952,74(5):5967-5970
|
被引
1
次
|
|
|
|
|
了解气象卫星更多信息，请访问