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ChemicalBook CAS DataBase List 2,3-Dichlorobenzaldehyde

2,3-Dichlorobenzaldehyde synthesis

8synthesis methods
-

Yield:6334-18-5 48.19 g

Reaction Conditions:

with hydrogen bromide;dihydrogen peroxide in 1,4-dioxane at 25; for 7 h;Temperature;

Steps:

1
In a 1L reactor,add 61.5 g of 2,3-dichlorotoluene, 3.075 g of azobisisobutyronitrile (5%), 215.25 g of 2-dichloroethane, heat the mixture at 75 ° C and add 44 g of bromine drop wise,reflux reaction till red bromine fades , Intermittent drip and 136.2g27.5% hydrogen peroxide continues to react till red bromine no longer generates. Add a 49.2g30% aqueous solution of sodium carbonate to the reaction solution, reflux reaction for 8 h ,at the same time recover1,2-dichloroethane.The hydrolyzate is heated and filtered at 80° C, into organic phase add 246g 1,4-Dioxane , add 40% of the catalyst HBr6.15g, add 27.5% hydrogen peroxide 38.3g,react at 25 ° C for 7 h. The reaction system is extracted three times with 1,2-dichloroethane,the organic phase is concentrated and obtained crude 2,3-dichlorobenzaldehyde, re-crystallization from ethanol and obtained 48.19 g of 2,3-dichlorobenzaldehyde, GC purity is 99.26% and yield is 72.1%.

References:

Lianyungang Industry Investment Group Co., Ltd.;Jiang Honglai;Jiang Xiao;Han Yong;Zang Han;Zhu Chengjie;Shen Weiwei CN107032968, 2017, A Location in patent:Paragraph 0015; 0017; 0018; 0019; 0022

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