These common heterocyclic compound, 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine, 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. Safety of (2,4-Dimethoxyphenyl)methanamine
Ethyl 4,6-dichloronicotinate (60 g, 0.27 mmol) at room temperatureDimethyl sulfoxide (500 ml)To the solution was added 2,4-dimethoxybenzylamine (47.8 g, 0.287 mmol)And triethylamine (55 g, 0.545 mmol) and the reaction mixture was stirred at room temperature overnight.To the reaction was added water (2 L), extracted with ethyl acetate (2.5 L x 2), washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo,Ethyl 6-chloro-4- (2,4-dimethoxybenzylamino) nicotinate was obtained.The product was dissolved in trifluoroacetic acid (300 ml), and the reaction mixture was stirred with heating at 50 C overnight. The mixture was cooled to room temperature and concentrated to dryness. The mixture was extracted with ethyl acetate (2.5 liters x 2), washed with brine (500 ml), and then the organic phase was washed with saturated aqueous sodium bicarbonate solution (500 ml). The organic phase was dried and concentrated in vacuo. The obtained product was purified by silica gel column chromatography (petroleum / ethyl acetate = 2/1) to obtain ethyl 4-amino-6-chloronicotinate (34 g, yield 62.3%) as a white solid. .
The synthetic route of (2,4-Dimethoxyphenyl)methanamine has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Nuowosida Pharmaceutical Co., Ltd.; Li Bing; (67 pag.)CN110256432; (2019); A;,
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