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ChemicalBook CAS DataBase List Ethyl 2-Aminoisonicotinate

Ethyl 2-Aminoisonicotinate synthesis

7synthesis methods
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Yield:13362-30-6 95.1%

Reaction Conditions:

with oxygen in water; pH=9 at 20 - 80; for 2 h;Reflux;Temperature;pH-value;

Steps:

1.2; 1.3; 2.2; 2.3; 3.2; 3.3 4.2; 4.3; 5.2; 5.3
(2) mixing 2-amino-4-methylpyridine with water, heating to 80 ° C, adding Cu-Ce-Bi-SiO 2 catalyst,After stirring, O2 was introduced into the solution, after completion of the reaction, the passage of O2 was stopped, and the temperature was lowered to room temperature, and the filtrate was adjusted to pH 9;
(3) After adding ethanol and heating to reflux for 2 hours, the ethanol was distilled off under reduced pressure, and the mixture was extracted with dichloromethane, and the organic phase was combined to remove dichloromethane to obtain ethyl 2-aminopyridine-4-carboxylate.
The molar ratio of copper nitrate, cerium nitrate and cerium nitrate in step (1) is 7:5:1;The mass ratio of cerium nitrate to nano SiO2 particles is 1:10, and the mass ratio of CTAB to nano SiO2 particles is 1:30.
In step (2), the mass ratio of 2-amino-4-methylpyridine to Cu-Ce-Bi-SiO2 catalyst is 14:3; the flow rate of O2 is 0.3 L/min.
The molar ratio of 2-amino-4-methylpyridine to ethanol in the step (3) is 1:1.1.The prepared 2-aminopyridine-4-carboxylic acid ethyl ester had a purity of 99.7% and a yield of 95.1%.

References:

Suzhou Gaide Careful Materials Co., Ltd.;Li Xiaoming CN109134361, 2019, A Location in patent:Paragraph 0020-0064

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