Ethyl 2-acetylisonicotinate synthesis
- Product Name:Ethyl 2-acetylisonicotinate
- CAS Number:25028-32-4
- Molecular formula:C10H11NO3
- Molecular Weight:193.2
1570-45-2
378 suppliers
$7.00/10g
123-63-7
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$40.60/100mL
25028-32-4
33 suppliers
$93.29/1g
Yield:25028-32-4 62%
Reaction Conditions:
with tert.-butylhydroperoxide;ferrous(II) sulfate heptahydrate;trifluoroacetic acid for 4 h;Reflux;
Steps:
Preparation of compound 1
CH3CN (180 mL), ethyl isonicotinate (19.2 g, 127 mmol)), paraldehyde (82 g, 620 mmol), FeSO4·7H2O (0.6 g, 2.16 mmol), TFA (14.86 g, 130 mmol), and 70% t-BuOOH (32 g, 252 mmol) was added into a 500 mL round bottom flask in sequence. The resulting mixture was heated to reflux for 4 h. After being cooled to room temperature, acetonitrile was removed in vacuum and the residue was neutralized. Then the as-obtained mixture was extracted with chloroform (3x100 mL). The combined organic fractions were dried over MgSO4, filtered and concentrated in vacuum followed by column chromatography (SiO2), eluting with the mixture of petroleum ether and ethyl acetate (13:1) to obtain the pure product, collected as a white solid (16 g, 62% yield).
References:
Bian, Rongrong;Ding, Xiaohui;Ge, Shuxian;Li, Mengying;Liao, Shengyun;Liu, Qiang;Su, Boya;Zhang, Haode;Zhu, Haitao [Inorganica Chimica Acta,2022,vol. 535,art. no. 120848] Location in patent:supporting information
55-22-1
621 suppliers
$5.00/5g
25028-32-4
33 suppliers
$93.29/1g