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ChemicalBook CAS DataBase List 1,2-Diethoxybenzene

1,2-Diethoxybenzene synthesis

11synthesis methods
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Yield:94-71-3 11.2 g ,2050-46-6 0.26 g

Reaction Conditions:

with zinc dibromide in tetralin at 240; under 7500.75 Torr; for 8 h;Autoclave;Green chemistry;Reagent/catalyst;Solvent;Temperature;Pressure;

Steps:

1-6 Example 2
In a 100 mL autoclave, Add 22.0 g (0.2 mol) of catechol, 49 g (50 mL) tetrahydronaphthalene, 1.0 g of cerium oxide and 0.1 g of zinc bromide, Cover the autoclave, Pump out most of the air in the kettle, Start heating and start stirring, when heating to 240 ° C, The ethylene gas is introduced to bring the pressure in the kettle to 1.0 MPa. Maintaining the reaction at this pressure for 8 hours; After the reaction is cooled to room temperature, Ethylene gas that is not involved in the reaction is released through a pressure reducing valve, The catalyst is recovered by filtration under reduced pressure; Then, most of the solvent tetrahydronaphthalene was removed by distillation under reduced pressure. The residue was separated by column chromatography to recover catechol (12.05 g, Conversion rate of raw materials is 45.2%), By-product o-ethoxyphenylethyl ether (0.26g), The finished o-ethoxyphenol finished product was 11.2 g (purity 99.1%, selectivity 97.7%).

References:

Shanghai Institute of Technology;Mao Haifang;Wang Hongchao;Zhang Wenxiang;Liu Jibo;Hu Xiaojun;Zhang Chiyuan CN109053396, 2018, A Location in patent:Paragraph 0023-0036

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