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ChemicalBook CAS DataBase List 2,3-Dimethylbenzoic acid
603-79-2

2,3-Dimethylbenzoic acid synthesis

11synthesis methods
-

Yield:603-79-2 81.3%

Reaction Conditions:

with 1-Butylimidazole;aluminum (III) chloride at 40; under 45004.5 Torr; for 48 h;Autoclave;Inert atmosphere;

Steps:

9 Example 9
Under an argon atmosphere, 40 mL of dry ortho-xylene was quickly added to a 250 mL PTFE-lined autoclave.2.5 g of anhydrous AlCl3, 1.16 g of dry N-butylimidazole, the reaction vessel was sealed after the addition was complete. Then connect the CO2 cylinder to the autoclave through the pipe, open the valve to control the CO2 pressure to 6MPa,At the same time stirring was turned on, the stirring rate was 1000 rpm, and finally heating was started and 48 hours at 40°C. After the reaction was completed, 150 mL of water was added to the reaction system, and the mixture was reacted for 30 min while stirring. After that, it was extracted 3 times with 50 mL of ether. The combined extracts were concentrated and dried to give 2.76 g of an off-white solid.The off-white solid was 2,3-dimethylbenzoic acid. The above-mentioned off-white solid was dissolved in 20 mL of a 10% wt sodium hydroxide solution, insolubles were filtered off, and a filtrate was obtained. Then, the filtrate was adjusted to pH 1 with 1 mol/L HCl and allowed to stand at room temperature for 60 min. Then it was transferred to -10°C and further crystallized and filtered to obtain crystals. The crystals were dried to give 2.29 g of 2,3-dimethylbenzoic acid as a white solid.The yield of 2,3-dimethylbenzoic acid was 81.3%.

References:

Shanxi Meiye Chemical Technology Institute Co., Ltd.;Wang Wentao;Tian Shidong;Qi Wenbo;Xue Qicai;Zhang Shengjun;Zheng Huaan;Yin Hailong CN107827742, 2018, A Location in patent:Paragraph 0059; 0060

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