These common heterocyclic compound, 37466-90-3, name is Ethyl 3,4-diaminobenzoate, 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. Computed Properties of C9H12N2O2
Preparation of ethyl 2-phenyl-1 H-benzo[d]imidazole-5-carboxylate 4-fluoro-3-nitrobenzoic acid (0.05g, 0.27 mmol) was esterified in the presence of catalytic sulfuric acid in ethanol (10mL) by refluxing at 65 eC for 6 hours. Ammonium hydroxide 28% (0.26 mmol) was subsequently added to the solution, stirred for 0.5 hour, treated with tin (Pi) chloride (190mg, 1 mmol) and stirred for a further 0.5 hour. The resulting mixture was then treated with benzaldehyde (0.3 mmol) and sodium bisulfite (57 mg, 0.3 mmol) and left to stir for another 3 hour. The solution was cooled to room temperature and subsequently evaporated under reduced pressure. It was resuspended in ethyl acetate (10mL), washed with 10% sodium carbonate (20mL) and water (20mL x2), dried over sodium sulfate and concentrated under reduced pressure. The crude products were purified by column chromatography (silica gel, 70- 230 mesh; C HC I3-MeOH 9:1 ) to obtain the final products (70-90%).
The synthetic route of Ethyl 3,4-diaminobenzoate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; UNIVERSITI SAINS MALAYSIA; OON, Chern Ein; TAN, Soo Choon; YEONG, Keng Yoon; ALI, Mohamed Ashraf; (39 pag.)WO2017/52359; (2017); A1;,
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