As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 94170-15-7, name is 1-Methyl-2-oxo-1,2-dihydropyridine-4-carbaldehyde, molecular formula is C7H7NO2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. COA of Formula: C7H7NO2
1- (1,1-dioxotetrahydro-2H-thian-4-yl) -6-((trans) -4-methylpyrrolidin-3-yl) -1,5-dihydro -4H-pyrazolo [3,4-d] pyrimidin-4-one trifluoroacetate (97mg, 0.21mmol, 1.0eq),1-methyl-2-oxo-1,2-dihydropyridine-4-carboxaldehyde (34.2 mg, 0.25 mmol, 1.2 eq)And acetic acid (25mg, 0.42mmol, 2.0eq) were dissolved in methanol (5mL), heated to 45 C for 2h,Cool down to 0 ,Add sodium cyanoborohydride (39.2 mg, 0.63 mmol, 3.0 eq) and stir at this temperature for 2 h.TLC monitoring showed no complete reaction,Additional 1-methyl-2-oxo-1,2-dihydropyridine-4-carboxaldehyde (114.3mg, 0.83mmol, 4.0eq) was added and stirred at this temperature for 2h,Add cyanoborohydride (39.2mg, 0.63mmol, 3.0eq), and react at 45 C for 2h.TLC monitoring showed complete reaction,Concentrated under reduced pressure, added saturated aqueous sodium carbonate (10 mL) and saturated brine (10 mL), and extracted with dichloromethane (50 mL x 4). The organic phases were combined, dried, filtered, and concentrated.The crude product was purified by preparative thin layer chromatography (MeOH: DCM = 1: 20)The product was obtained as an off-white solid (59 mg, yield: 45.6%).
With the rapid development of chemical substances, we look forward to future research findings about 94170-15-7.
Reference:
Patent; Nanjing Yaojie Good Health Biological Technology Co., Ltd.; Wu Yongqian; Peng Peng; Li Lin; (59 pag.)CN110357888; (2019); A;,
Pyridine – Wikipedia,
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