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. 201937-23-7, name is 6-Chloronicotinimidamide hydrochloride. A new synthetic method of this compound is introduced below., name: 6-Chloronicotinimidamide hydrochloride
2-(6-chloropyridin-3-yl)-4-(2-methoxyethoxy)-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine (O-l) A suspension of 1-tert-butyl 3 -ethyl 4-oxopiperidine-l,3-dicarboxylate (A-I, 41.5 g, 153 mmol), -chloropyridine-S-carboximidamide hydrochloride (43.9 g, -85% pure, 194 mmol), and K2CO3 (59.8 g, 433 mmol) in DMF (457 mL) was treated with 2-bromoethyl methyl ether (26.3 ml, 280 mmol) with stirring. The mixture was heated to 65 ºC and stirred for 24 hr, adding additional small equivalents of 2-bromoethyl methyl ether and K2CO3 to drive reaction to completion if needed. The reaction mixture was diluted with EtOAc (1.5 L), and washed with water (2 L), sat. aq. NaHCO3 (2 L), water (2 L), and brine (1 L). The organic phase was dried over Na2SO4, filtered, and concentrated in vacuo to provide unpurified Boc-protected intermediate (~62 g), which was used in the subsequent step without further purification.
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Reference:
Patent; MERCK SHARP &; DOHME CORP.; BRESLIN, Michael, J.; COLEMAN, Paul, J.; COX, Christopher, D.; RAHEEM, Izzat, T.; SCHREIER, John, D.; WO2010/138430; (2010); A1;,
Pyridine – Wikipedia,
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