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ChemicalBook CAS DataBase List 2-Acetamino-4-aminopyridine
75279-39-9

2-Acetamino-4-aminopyridine synthesis

8synthesis methods
Acetamide, N-(4-nitro-2-pyridinyl)-, oxide (9CI)

4487-48-3

2-Acetamino-4-aminopyridine

75279-39-9

The general procedure for the synthesis of N-(4-aminopyridin-2-yl)acetamide from the compound (CAS: 4487-48-3) was as follows: iron powder (140 g, 2.5 mol) was added to a 1 L four-necked reaction flask, followed by the addition of acetic acid (458 mL, 8 mol) and 100 mL of water. The mixture was heated to reflux for 15 min and then cooled to 85 °C to give compound c (197 g, 1 mol). Due to the exothermic nature of the reaction, heating and refluxing was continued for 2 h to ensure complete reaction, after which it was cooled to room temperature. The solid residue was removed by suction filtration and the filtrate was washed with an appropriate amount of solvent. The filtrates were combined and 2 g of antioxidant powder was added to protect the product from oxidation. The filtrate was subjected to rotary evaporation to afford the solid compound d (139.2 g, 92.2% yield).

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Yield:75279-39-9 92.2%

Reaction Conditions:

with iron;acetic acid in water; for 2 h;Reflux;

Steps:

4 Preparation of 2-acetamido-4-aminopyridine

Iron powder (140g, 2.5mol) will be reducedPut acetic acid (458ml, 8mol) and 100mL water into a 1L four-mouth reaction flask.Heat reflux 15min,Cool to 85°C,Compound c (197 g, 1 mol) was added slowly,The reaction is exothermic,After the addition of heat reflux 2h,The reaction is completeCool to room temperatureSuction filtrationFilter residue washed,Combine the filtrate,Add 2g of powder to the filtrate,To prevent the product from being oxidized,Before proceeding with the next reaction,Rotary evaporation of the solution gave solid compound d (139.2 g, 92.2%).

References:

CN107759515,2018,A Location in patent:Paragraph 0035-0037