Preparation method of 5-bromo-2-chlorobenzoic acid
A technology of chlorobenzoic acid and aminobenzoic acid, which is applied in the preparation of carboxylate, organic compound, and cyanide reaction, etc., can solve the problems of unfavorable industrial production, long reaction time, and high environmental pressure, and achieve effective Benefits of industrial production, short production cycle, high yield and purity
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Embodiment 1
[0041] Add 2-nitrobenzoic acid (50g, 0.299mol) into dichloromethane (200mL), stir, add thionyl chloride (42.7g, 0.359mol), heat up to reflux temperature, reflux for 5 hours, the remaining raw materials < 1%, stop the reaction; drop the temperature below 5°C, add methanol (15g, 0.469mol) dropwise, control the temperature below 10°C during the dropwise addition, stir for 30 minutes after the dropwise addition, and concentrate under reduced pressure at 40°C to obtain light Yellow liquid methyl 2-nitrobenzoate (first intermediate) 48.8g, yield 90%, purity 99.2%.
Embodiment 2
[0043] Add 2-nitrobenzoic acid (50g, 0.299mol) into methanol (200mL), stir, cool down to 0-5°C, add thionyl chloride (42.7g, 0.359mol) dropwise, after the dropwise addition, in React at a temperature of 0-5°C for 1 hour. After the reaction is completed, slowly raise the temperature to reflux temperature and react at reflux for 2 hours. If the remaining raw materials are <1%, stop the reaction and concentrate under reduced pressure at 40°C to obtain 2- Methyl nitrobenzoate (first intermediate) 49.3g, yield 91%, purity 99.3%.
Embodiment 3
[0045] Add 2-nitrobenzoic acid (50g, 0.299mol) into toluene (200mL), stir, add anhydrous magnesium sulfate (20g), ethanol (22g, 0.478mol), heat up to reflux temperature, and reflux for 7 hours. <1% of the raw material remained, the reaction was stopped, filtered, and the filtrate was concentrated under reduced pressure to obtain 51.3 g of ethyl 2-nitrobenzoate (the first intermediate) as a light yellow liquid, with a yield of 87.8% and a purity of 99.6%.
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