摘要
以3，5-二硝基苯甲酰氯、3-氨基丙酸和6-氨基正己酸为原料，室温反应合成了3．（3，5-二硝基苯甲酰氨基）丙酸和6-（3，5-二硝基苯甲酰氨基）正己酸。反应过程中，3，5-二硝基苯甲酰氯分批加入，滴加2mol／L氢氧化钠水溶液控制反应体系的pH=8—9，n（3，5-二硝基苯甲酰氯）／n（氨基酸）=1，收率分别为84％和81％；硝基化合物经10％钯炭催化剂（用量为反应物质量的10％）催化加氢，再经盐酸酸化，得目标产物3-（3，5-二氨基苯甲酰氨基）丙酸盐酸盐和6-（3，5-二氨基苯甲酰氨基）正己酸盐酸盐，收率分别为93％和94％。相关化合物的结构通过FTIR、^1HNMR、^13CNMR进行了表征。
3-（3, 5-Dinitrobenzoylamido ） propanoic acid （ Ⅰ ） and 6-（ 3,5-dinitrobenzoylamido ） hexanoic acid （ Ⅱ ） were synthesized respectively by reaction of 3,5-dinitrobenzoyl chloride with 3- aminopropanoic acid and 6-aminohexanoic acid at room temperature. In the experiment, 3, 5- dinitrobenzoyl chloride should be added in portions,2 mol/L aqueous NaOH solution was dropped into the reaction system to keep pH = 8 -9, and n（3,5-dinitrobenzoyl chloride） ：n（ amino acid） = 1. Yields of Ⅰ and Ⅱ are 84% and 81% respectively. The nitro compounds Ⅰ and Ⅱ were hydrogenated with 10% Pd /C as catalyst [ m （ catalyst ） ： m （ nitro compound ） = 10 ： 100 ], and then acidized with hydrochloric acid to get the title compounds 3-（3, 5-diaminobenzoylamido ）propanoic acid hydrochloride and 6-（3,5-diaminobenzoylamido） hexanoic acid hydrochloride in 93% and 94% yield respectively. Structures of the compounds were confirmed by FTIR, ^1HNMR and ^13CNMR.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2006年第12期1161-1163,共3页
Fine Chemicals
基金
国家自然科学基金资助项目(20573049)~~
