ChemicalBook CAS DataBase List 5-BROMO-2-CHLORO-BENZOYL CHLORIDE

5-BROMO-2-CHLORO-BENZOYL CHLORIDE synthesis

5synthesis methods

Product Name:5-BROMO-2-CHLORO-BENZOYL CHLORIDE
CAS Number:21900-52-7
Molecular formula:C7H3BrCl2O
Molecular Weight:253.91

5781-53-3 Synthesis

5781-53-3
215 suppliers
$8.00/10g

106-39-8 Synthesis

106-39-8
442 suppliers
$14.00/5g

21900-52-7
78 suppliers
$12.00/250mg

Yield: 98.9%

Reaction Conditions:

Stage #1:monomethyl oxalyl chloride with copper sulfate supported molecular sieve in 1,1,1-trichloroethane at 125; under 4560.31 Torr; for 1.5 h;Inert atmosphere;
Stage #2:bromochlorobenzene in chloroform;1,1,1-trichloroethane at 165; under 6080.41 Torr; for 14 h;Inert atmosphere;Temperature;Pressure;

Steps:

1-8 A method for synthesizing 5-bromo-2-chlorobenzoyl chloride, comprising the steps of:
Mix oxalyl chloride monomethyl ester with 1,1,1-trichloroethane, add catalyst, stir and pass argon gas, control the pressure to 6 atmospheres, control the temperature to 125 ° C, maintain 1.5 h, Then, a solution of 4-bromochlorobenzene and chloroform was added dropwise, and after the addition, the temperature of the system was raised to 165 ° C, and the pressure was raised to 8 atm to continue the reaction for 14 hours.The catalyst is obtained by grinding the 4A molecular sieve, after 350 mesh, immersing in a 12% mass fraction of copper sulfate aqueous solution for 4 days, filtering, and baking at 400 ° C to obtain the weight ratio of molecular sieve to copper sulfate aqueous solution; It is 1:7.2.The molar ratio of 4-bromochlorobenzene to oxalyl chloride monomethyl ester is 1:1.12; the ratio of oxalyl chloride monomethyl ester to 1,1,1-trichloroethane is lg: 11ml; 4-bromochlorobenzene and chloroform The dosage ratio is lg: 8 ml; the weight ratio of 4-bromochlorobenzene to the catalyst is 1:1.15.2) After cooling, the solid was removed by filtration, and the filtrate was added to a volume of 1 to 2 volumes of toluene, washed with water to pH = 7. The mixture was dried over anhydrous sodium sulfate and evaporated to give a product. The molar yield was 98.9%, and the GC purity was 99.1%.

References:

Shenzhen The Second People Hospital;Tan Hui;Li Weiping;Huang Xianjian;Tang Aifa;Liu Wenlan;Chen Lei CN109456177, 2019, A Location in patent:Paragraph 0031-0059

21739-92-4 Synthesis