利用芳香胺的重氮化-偶合显色反应原理,建立了纺织品中24种禁用芳香胺的快速定性筛选测定方法。样品经还原后,先用10 mL叔丁基甲醚萃取,再用5 mL HCl反萃取,达到净化和脱色的目的,HCl萃取液中加入0.05 mL NaNO2,重氮化反应10 min,滴加0....利用芳香胺的重氮化-偶合显色反应原理,建立了纺织品中24种禁用芳香胺的快速定性筛选测定方法。样品经还原后,先用10 mL叔丁基甲醚萃取,再用5 mL HCl反萃取,达到净化和脱色的目的,HCl萃取液中加入0.05 mL NaNO2,重氮化反应10 min,滴加0.5 mL氨基磺酸铵除去多余的NaNO2,加入1mL邻甲氧基苯酚与重氮盐偶联显色。根据萃取液是否显色,快速地对样品中是否含有禁用偶氮染料作出初步判断。方法的检出限低于15 mg/kg,上千个实际样品测试无假阴性,假阳性概率为28%。本方法无需大型色谱仪器设备,与仪器测定方法相比,前处理时间缩短了约60%,节约了约90%的试剂费用。展开更多
A novel carbonyl transposition reaction led by aromatic amines nucleophilic addition to \{2 oxo glycoside\} was discovered. The mechanism of the reaction was provided through tracing the change of 1H NMR of a hemiacet...A novel carbonyl transposition reaction led by aromatic amines nucleophilic addition to \{2 oxo glycoside\} was discovered. The mechanism of the reaction was provided through tracing the change of 1H NMR of a hemiacetal intermediate which was obtained in the reaction of o phenylene diamine with 2 oxo glycoside. Both the intermediate and the product were identified by FTIR, 1H NMR, 13 C NMR, 1H 1H COSY and 1H 13 C COSY spectra. The other aromatic amines reaction with 2 oxo glycoside also proved the mechanism. This reaction provides a new method for preparing 2 deoxy 2 aromatic amino 3 oxo glycosides, which is a new kind of material used in assymetric synthesis.展开更多
室温条件下,对氨基苯磺酸铝可有效催化苯乙酮、芳香醛和芳香胺的Mannich反应,三组分＂一锅法＂合成了系列β-氨基酮衍生物.考察了反应条件对收率的影响及对氨基苯磺酸铝对不同底物Mannich反应的催化效果,推测了反应机理.产物结构经IR、^...室温条件下,对氨基苯磺酸铝可有效催化苯乙酮、芳香醛和芳香胺的Mannich反应,三组分＂一锅法＂合成了系列β-氨基酮衍生物.考察了反应条件对收率的影响及对氨基苯磺酸铝对不同底物Mannich反应的催化效果,推测了反应机理.产物结构经IR、^1 H NMR和质谱进行表征.合成不同的β-氨基酮衍生物的较佳反应条件为：苯乙酮、芳香醛和芳香胺物质的量比为1.1：1：1,对氨基苯磺酸铝用量为苯甲醛物质的量的3%,乙醇用量5 mL.该方法操作简单,条件温和,收率高,催化剂可重复使用,对环境友好.展开更多
文摘利用芳香胺的重氮化-偶合显色反应原理,建立了纺织品中24种禁用芳香胺的快速定性筛选测定方法。样品经还原后,先用10 mL叔丁基甲醚萃取,再用5 mL HCl反萃取,达到净化和脱色的目的,HCl萃取液中加入0.05 mL NaNO2,重氮化反应10 min,滴加0.5 mL氨基磺酸铵除去多余的NaNO2,加入1mL邻甲氧基苯酚与重氮盐偶联显色。根据萃取液是否显色,快速地对样品中是否含有禁用偶氮染料作出初步判断。方法的检出限低于15 mg/kg,上千个实际样品测试无假阴性,假阳性概率为28%。本方法无需大型色谱仪器设备,与仪器测定方法相比,前处理时间缩短了约60%,节约了约90%的试剂费用。
文摘A novel carbonyl transposition reaction led by aromatic amines nucleophilic addition to \{2 oxo glycoside\} was discovered. The mechanism of the reaction was provided through tracing the change of 1H NMR of a hemiacetal intermediate which was obtained in the reaction of o phenylene diamine with 2 oxo glycoside. Both the intermediate and the product were identified by FTIR, 1H NMR, 13 C NMR, 1H 1H COSY and 1H 13 C COSY spectra. The other aromatic amines reaction with 2 oxo glycoside also proved the mechanism. This reaction provides a new method for preparing 2 deoxy 2 aromatic amino 3 oxo glycosides, which is a new kind of material used in assymetric synthesis.
文摘室温条件下,对氨基苯磺酸铝可有效催化苯乙酮、芳香醛和芳香胺的Mannich反应,三组分＂一锅法＂合成了系列β-氨基酮衍生物.考察了反应条件对收率的影响及对氨基苯磺酸铝对不同底物Mannich反应的催化效果,推测了反应机理.产物结构经IR、^1 H NMR和质谱进行表征.合成不同的β-氨基酮衍生物的较佳反应条件为：苯乙酮、芳香醛和芳香胺物质的量比为1.1：1：1,对氨基苯磺酸铝用量为苯甲醛物质的量的3%,乙醇用量5 mL.该方法操作简单,条件温和,收率高,催化剂可重复使用,对环境友好.
