Electric Literature of 870997-87-8, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 870997-87-8, name is 2-Amino-N-methylnicotinamide. A new synthetic method of this compound is introduced below.
Example 1, Step A, Method A and Method B; A 500 ml round bottomed flask was charged with methyl 2- aminopyridine 3-carboxamide 1 (4.5 g, 29.76 mmol) and 1 ,2-dichloroethane(150 ml). The resulting solution was cooled to -40 C while triphosgene (7 g,23.59 mmol) was slowly added. Triethylamine (4.4 g, 43.48 mmol) was then added via a syringe dropwise at this temperature. The reaction mixture was stirred at -40 C for two hours before warming up gradually to room temperature and maintained at this temperature overnight. The suspension was treated with water (100 ml) and saturated sodium carbonate (100 ml) and separated. The aqueous solution was extracted with dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated on rotavapor. The residue was dried under house vacuum to provide a deep tan solid (4.1 g). This material was mixed with phosphorus oxychloride (50 ml) in a 250 ml flask. The resulting suspension was refluxed for 4 hours. The excess phosphorus oxychloride was removed by distillation under reduced pressure. The residue was dissolved in methylene dichloride (200 ml) and poured into ice (50 g). The suspension was neutralized with saturated sodium carbonate solution and separated. The organic layer was dried over sodium sulfate, concentrated, and dried under vacuum to afford a black gel (1.4 g), which was used directly for the next reaction without purification.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,870997-87-8, 2-Amino-N-methylnicotinamide, and friends who are interested can also refer to it.
Reference:
Patent; SCHERING CORPORATION; PHARMACOPEIA, INC.; WO2008/79279; (2008); A1;,
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