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ChemicalBook CAS DataBase List 4-CHLORO-2-NITROPHENOL
89-64-5

4-CHLORO-2-NITROPHENOL synthesis

9synthesis methods
2,5-Dichloronitrobenzene is hydrolyzed with 8 % aqueous sodium hydroxide at 120 – 130 ℃ under pressure.
-

Yield:89-64-5 62%

Reaction Conditions:

with water in tetrahydrofuran at 25; for 2.5 h;Schlenk technique;

Steps:

(A) Typical Experimental Procedure for the Radical Coupling Reaction:
General procedure: To a Schlenk tube were added Phenol 1 (0.3 mmol), tert-Butyl nitrite 2a (0.6mmol), H2O (0.6 mmol), and THF (2 mL). Then the tube was stirred at 25 oC under airatmosphere for the indicated time until complete consumption of starting materialmonitored by TLC analysis. After the reaction was finished, the organic extracts weredried over anhydrous Na2SO4, concentrated in vacuum, and the resulting residue waspurified by silica gel column chromatography (hexane/ethyl acetate) to afford thedesired product 3.

References:

Wei, Wen-Ting;Zhu, Wen-Ming;Liang, Weida;Wu, Yi;Huang, Hui-Yan;Huang, Yi-Ling;Luo, Junfei;Liang, Hongze [Synlett,2017,vol. 28,# 16,p. 2153 - 2156] Location in patent:supporting information

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