ChemicalBook CAS DataBase List 2,6-Difluorophenol

2,6-Difluorophenol synthesis

10synthesis methods

Product Name:2,6-Difluorophenol
CAS Number:28177-48-2
Molecular formula:C6H4F2O
Molecular Weight:130.09

2,6-Difluorophenol can be used as organic synthesis intermediates and pharmaceutical intermediates, mainly in laboratory research and development. It was prepared from 2,6-difluoroanisole and sodium iodide by stirring in acetonitrile for 5 h at room temperature.

5509-65-9
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$10.00/10g

28177-48-2
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$15.00/5 g

Yield:28177-48-2 88.9%

Reaction Conditions:

Stage #1:2,6-difluoroaniline with sulfuric acid;sodium nitrite in water at -5 - 0; for 2 h;Green chemistry;Large scale;
Stage #2: with sulfuric acid;copper(II) sulfate in waterReflux;Green chemistry;Large scale;Reagent/catalyst;Temperature;

Steps:

1.2; 2-8 (2) Preparation of aqueous phase of 2,6-difluorophenol:
25 kg of prepared 30% aqueous sulfuric acid solution was added to the reactor and3.0 kg (23 mol) of 2,6-difluoroaniline, heated under stirring,Completely dissolve 2,6-difluoroaniline and cool to -5 °C with vigorous stirring.Then slowly add 5.6 kg of prepared 30% sodium nitrite solution.Maintain the reaction temperature at -5 to 0 ° C, continue to react for 2 h after the addition, filter, discard the filter residue, decompose excess nitrous acid with aqueous urea solution, and adjust to the starch blue potassium iodide test paper.The 2,6-difluoroaniline diazonium salt aqueous solution was directly stored in the following reaction.Adding to a mixture of 22 kg of a 50% aqueous solution of sulfuric acid and 4.0 kg of copper sulfate in a separate kettle under reflux, and distilling while dropping, the resulting 2,6-difluorophenol is promptly transferred and distilled. The liquid was separated, dried, filtered, and evaporated under reduced pressure to give white product 2, 6-difluoro phenol with a purity of 98.6% and a yield of 88.9%.

References:

Ludong University;Liu Gang;Wang Haojie;Wang Jinming;Ren Yujin;Zhang Yuchun;Mu Xianfeng;Zhu Fei;Wang Shengjie;Han Qinglin;Xu Guanhua CN109456225, 2019, A Location in patent:Paragraph 0010; 0013; 0014; 0017-0023

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437-82-1 Synthesis