C.I.溶剂黄21清洁合成工艺的研究

The Development of Clean Technological Process for Synthesizing C.I.Solvent Yellow 21

邻氨基苯甲酸在0℃-5℃重氮化,与1-苯基-3-甲基-5-吡唑啉酮偶合得单偶氯染料,研究了水和三乙醇胺(45.1)为混合溶剂取代高毒的DMF,以甲酸铬为络合剂,在90℃-95℃络合反应2小时,合成了标题染料经TLC、IR、HPLC分析,主要杂质为1:1型络合染料。

C.I. solvent yellow 21 was synthesized by diazotizing o-aminobenzoic acid at 0-5 ℃ and coupling with l-phenyl-3-methyl-5-pyrazolone to give a monoazo dyes, then complexed with chromium formate at 90-95 for 2h in a mixture of water and triethanolamine (H2O: (HOCH2CH2)3N=4.5:1) instead of DMF as solvent. Analyzed by TLC, IR and HPLC, the main impurity was 1:1 chromium complex dye.