N-苯基-2,4-二氯苯胺合成与表征

Synthesis and Characterization of 2,4-Dichloro-N-Phenyl Benzenamine

以苯胺、氯乙酰氯和2,4-二氯苯酚为原料,吡啶为酰化的酸缚剂,碳酸钾为酚的缩合反应催化剂,氢氧化钠为Smiles重排反应的催化剂,在反应物料配比为n(苯胺):n(氯乙酰氯):n(吡啶):n(碳酸钾):n(氢氧化钠)=1:1.1:1.2:0.9:1.3,重排反应温度105℃,时间10h,通过酰化、缩合、重排、水解四步"一锅烩"的办法合成了N-苯基-2,4-二氯苯胺,收率为60%,产物结构通过IR、NMR和元素分析进行了确认。

2,4- dichloro- N - phenyl benzenamine was synthesized by Smiles rearrangement in one pot in yields 60 % using aniline, 2, 4 - dichloride phenol and chloroacetyl chloride as starting materials in the presence of pyridine as acid - bonding agent, potassium carbonate as condensation catalyst, sodium hydroxide as rearrangement catalyst in the molar ratio of aniline to chloroacetyl chloride to pyridine to potassium carbonate to sodium hydroxide of 1 ： 1 . 1 ： 1 . 2 ： 0.9 ： 1 . 3. The rearrangement reaction temperature and time were at 105 ℃, 10h, respectively. The structure of title compound was confirmed by IR, NMR spectra and elemental analysis.