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4,4'-(1,3-Phenylenebisoxy)bis(1-nitrobenzene) synthesis

4synthesis methods
-

Yield: 76%

Reaction Conditions:

with urea;zinc(II) chloride in neat (no solvent) at 80; for 2.5 h;Green chemistry;Ullmann Condensation;

Steps:

General procedure for preparation of symmetrical arylether dinitromonomer (3a~3l):
General procedure: A mixture of aryl halide (2 mmol), dihydroxy compound(1 mmol) and 4 Urea/ZnCl2 (5% DES/NMP), as a catalyst,was stirred in a 100 ml round bottom flask with a condenser on the top. The mixture has been stirred for 2-3 h. It was slowly warmed up to 80 °C. The progress of the reaction was monitored by HTLC (mobile phase = Methanol:Water =80:20). After completing the reaction, deionized water (50mL) were added and the mixture was stirred for 30 min. The crude product was extracted from organic phase by ethylacetate and recrystallized from ethanol to obtain the pure product. The DES catalyst was recycled and used without further purification.

References:

Jin, Yan;Ding, Yinhao;Hou, Xichao;Dong, Jingjing;Lu, Jianqiang;Feng, Baicheng [Journal of the Indian Chemical Society,2020,vol. 97,# 1,p. 101 - 107]

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