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ChemicalBook CAS DataBase List Trimethylphloroglucinol
4463-03-0

Trimethylphloroglucinol synthesis

6synthesis methods
-

Yield:4463-03-0 82.3 %

Reaction Conditions:

in water at 60 - 100;

Steps:

4.2. General Procedure for the Hydrolysis of the Sulfuric-Acid Salts of TriaminobenzeneDerivatives 2b-d

General procedure: Into a round-bottom flask equipped with a reflux condenser, a magnetic stirrer, and athermometer were placed distilled water (50 mL) and sodium sulfite (50 mg). Compound 2(5 g) was added to the solution at 60 C with stirring. The reaction mixture was refluxedfor the required time. After the reaction was complete, the reaction mixture was filtered ashot and the filtrate was cooled to 20-25 C. The filtrate was then saturated with sodiumchloride, and the product was extracted with ethyl acetate or diethyl ether (4 15 mL) andwashed with brine (5 mL). The extract was dried over Na2SO4 and the solvent was thenremoved in vacuo.Procedure A: reaction mixture refluxed for 24 h and 3b extracted with ethyl acetate.Procedure B: reaction mixture refluxed for 35 h and 3c extracted with diethyl ether.Procedure C: reaction mixture refluxed for 14 h and 3d extracted with ethyl acetate.

References:

Shchurova, Irina A.;Alekseyeva, Natalia A.;Sysolyatin, Sergey V.;Malykhin, Valeriy V. [Molecules,2022,vol. 27,# 23,art. no. 8595]

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