Коллеги, у кого есть возможность, помогите пожалуйста с поиском метода синтеза соединения:
CCOC(=O)C(=O)c1c(C)c(Cl)cc(C)c1Cl
Спасибо!
+++поиск метода синтеза
+++поиск метода синтеза
Последний раз редактировалось bromin Ср апр 16, 2025 4:24 am, всего редактировалось 1 раз.
Re: поиск метода синтеза
есть только получ метилового эфира
из Methyl oxalyl chloride и 1,4-dichloro-2,5-dimethylbenzene
With aluminum (III) chloride In 1,2-dichloro-ethane at 20 - 75℃; Solvent; Temperature;
Experimental Procedure
94 %
Current Patent Assignee: BEIJING BIOLIGO BIOTECHNOLOGY - CN116606271, 2023, A
Location in patent: Paragraph 0031; 0033-0039
Abstract
1-2 Example 2 Synthesis of methyl 2-(2,5-dichloro-3,6-dimethylphenyl)-2-oxoacetate (Formula III, R=methyl)
Add 100.0mL of dichloroethane to a 250mL reaction flask that has been cleanly dried, equipped with a drying tube and an exhaust gas absorption device, and add 25.0g of 2,5-dichloroparaxylene (Formula I) and 40.0g of aluminum trichloride at room temperature with stirring. Under stirring, slowly add 36.8g of oxaloyl chloride monomethyl ester (formula II, R = methyl), and the reaction system is maintained at 35~75 °C to continue the reaction until the raw materials are consumed. After the reaction, the reaction solution was cooled to room temperature, poured into 250g of ice water to fully quench, and 150mL of dichloroethane was added to extract. The organic phase was collected, washed with 250mL of 15% ammonium chloride aqueous solution and 250mL of saturated sodium bicarbonate aqueous solution, and then dried with 25g of anhydrous sodium sulfate, and 2-(2,5-dichloro-3,6-dimethylphenyl)-2-oxylineacetate methyl ester (formula III, R=methyl) was obtained by filtration, washing and removal of solvent, with a yield of 94.0% and a purity of 95.5% HPLC. Similar results can be obtained when R is ethyl.
из Methyl oxalyl chloride и 1,4-dichloro-2,5-dimethylbenzene
With aluminum (III) chloride In 1,2-dichloro-ethane at 20 - 75℃; Solvent; Temperature;
Experimental Procedure
94 %
Current Patent Assignee: BEIJING BIOLIGO BIOTECHNOLOGY - CN116606271, 2023, A
Location in patent: Paragraph 0031; 0033-0039
Abstract
1-2 Example 2 Synthesis of methyl 2-(2,5-dichloro-3,6-dimethylphenyl)-2-oxoacetate (Formula III, R=methyl)
Add 100.0mL of dichloroethane to a 250mL reaction flask that has been cleanly dried, equipped with a drying tube and an exhaust gas absorption device, and add 25.0g of 2,5-dichloroparaxylene (Formula I) and 40.0g of aluminum trichloride at room temperature with stirring. Under stirring, slowly add 36.8g of oxaloyl chloride monomethyl ester (formula II, R = methyl), and the reaction system is maintained at 35~75 °C to continue the reaction until the raw materials are consumed. After the reaction, the reaction solution was cooled to room temperature, poured into 250g of ice water to fully quench, and 150mL of dichloroethane was added to extract. The organic phase was collected, washed with 250mL of 15% ammonium chloride aqueous solution and 250mL of saturated sodium bicarbonate aqueous solution, and then dried with 25g of anhydrous sodium sulfate, and 2-(2,5-dichloro-3,6-dimethylphenyl)-2-oxylineacetate methyl ester (formula III, R=methyl) was obtained by filtration, washing and removal of solvent, with a yield of 94.0% and a purity of 95.5% HPLC. Similar results can be obtained when R is ethyl.
Re: поиск метода синтеза
mishka, большое спасибо за Вашу работу
Надеялся, что в базах побогаче с информацией будет

Надеялся, что в базах побогаче с информацией будет

Кто сейчас на конференции
Сейчас этот форум просматривают: ineosA и 10 гостей