3-Acetoacetylpyridine synthesis
- Product Name:3-Acetoacetylpyridine
- CAS Number:3594-37-4
- Molecular formula:C9H9NO2
- Molecular Weight:163.17
Yield:3594-37-4 81%
Reaction Conditions:
with sodium hydride in N,N-dimethyl-formamide at 0 - 20;Inert atmosphere;
Steps:
1
0 °C lower, round bottom flask is added sodium hydride (1.8 g) and nicotinic acid methyl ester (5.0 g) in DMF (29 ml) solution, under the protection of argon, dropping acetone (3.2 ml) in DMF (12 ml) solution. Then the reaction mixture temperature to room temperature, stirring for several hours, TLC tracking the reaction until the completion of the reaction. Reaction solution 1.0 M HCl to adjust the pH 5 - 6, will be precipitated and filtered, the filtrate diluted with water and ethyl acetate. Separation of the aqueous phase is extracted with ethyl acetate three times, the combined organic phase with saturated salt water washing, drying with anhydrous sodium sulfate, concentrated, for PE/EA (20:1 - 3:1) as the mobile phase, column chromatography [...] condensation product (4.8 g, 81%).
References:
CN108329325,2018,A Location in patent:Paragraph 0046-0048
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