ChemicalBook CAS DataBase List 3,4-Dichlorobenzoic acid

3,4-Dichlorobenzoic acid synthesis

12synthesis methods

Product Name:3,4-Dichlorobenzoic acid
CAS Number:51-44-5
Molecular formula:C7H4Cl2O2
Molecular Weight:191.01

1805-32-9
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$8.00/5g

51-44-5
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$6.00/10g

Yield:51-44-5 96.8%

Reaction Conditions:

with Au NCs/TiO₂;oxygen;sodium hydroxide in water at 120; under 7500.75 Torr; for 6 h;Autoclave;Green chemistry;

Steps:

General procedure: The oxidation of alcohols was performed in an autoclave reactor equipped with a magnetic stirrer, thermocouple, automatic temperature controller and a pressure gauge. After the addition of desired amount of reactant, catalyst, water and NaOH, the autoclave was sealed. The atmosphere over the mixture was replaced with O₂ for three times. Then the reactor was heated to the desired temperature with stirring. Subsequently, the pressure of O₂ was charged to 1.0 MPa and kept constant during the reaction through feeding O₂. When the reaction was finished, the reactor was cooled down to the ambient temperature. The reaction mixture was diluted with acetone to dissolve the products. After the catalyst was separated, the filtrate was acidified to pH of 2.0 by hydrochloric acid. The oxidation products were analyzed by gas chromatography equipped with a flame ionization detector. The isolated yield of carboxyl acid was obtained with the following procedure. The solvent of the mixture after acidification was removed through rotary evaporation. The pH of the residual was adjusted to 10.0 with NaOH (2.0 M), and then it was extracted with ethyl acetate for three times. The aqueous layer was acidified to pH 2.0 using HCl (6.0 M) and extracted with ethyl acetate. The organic layer was removed ethyl acetate through rotary evaporation to get the carboxylic acid. The carboxylic acid was dried overnight for calculation of the isolated yield.

References:

Zhou, Lipeng;Chen, Minzhu;Wang, Youqiang;Su, Yunlai;Yang, Xiaomei;Chen, Chen;Xu, Jie [Applied Catalysis A: General,2014,vol. 475,p. 347 - 354]

95-75-0 Synthesis