Electric Literature of 1949-51-5, A common heterocyclic compound, 1949-51-5, name is Ethyl 3,5-diaminobenzoate, molecular formula is C9H12N2O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
In a round-bottom flask placed in an ice bath, 11 (1.0 eq.) was solubilized in a mixture of dioxane and water (2:1), followed by addition of triethylamine (Et3N; 2.2 eq.). Next, di-tert-butyl-dicarbonate ((Boc)2O; 1.0 eq.) was solubilized in a small amount of dioxane and added dropwise to the mixture. The reaction was stirred at room temperature overnight. The solvents were evaporated and the crude was dissolved in ethyl acetate and washed with 10% aqueous solution of citric acid and water. The collected organic phases were dried over MgSO4, concentrated in vacuo and purified by column chromatography (dichloromethane/acetonitrile 95/5-90/10). The desired product formed pale-yellow crystals (80% yield).
The synthetic route of 1949-51-5 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Czescik, Joanna; Zamolo, Susanna; Darbre, Tamis; Mancin, Fabrizio; Scrimin, Paolo; Molecules; vol. 24; 15; (2019);,
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