Preparation method of 5-amino-2-pyridinecarboxamide Background and overview of rubidium carbonate
5-Amino-2-pyridinecarboxamide can be used as a pharmaceutical and chemical synthesis intermediate. If 5-amino-2-pyridinecarboxamide is inhaled, move the patient to fresh air; if skin contact occurs, remove contaminated clothing and rinse skin thoroughly with soap and water, if any If you feel discomfort, seek medical attention; if eye contact occurs, separate eyelids, rinse with running water or saline, and seek medical attention immediately; if ingested, rinse mouth immediately, do not induce vomiting, and seek medical attention immediately.
Preparation method of 5-amino-2-pyridinecarboxamide
Method 1: Preparation of 5-amino-2-pyridinecarboxamide, which is prepared by hydrolysis reaction using 5-amino-pyridine-2-carbonitrile as raw material. The reaction equation is as follows:
The specific steps are: add a mixture of 30% H2O2 (1ml), 3N NaOH (3ml) and 3ml NaOH into an 18ml vial. To the mixture was added 5-amino-pyridine-2-carbonitrile (450 mg, 3.78 mmol) at room temperature. The reaction mixture was stirred at room temperature for 45 minutes and TLC showed consumption of starting material. The mixture was diluted with water and filtered; the solid was washed with water and dried to give 480 mg of 5-amino-2-pyridinecarboxamide product in 92% yield.
Method 2: The preparation of 5-amino-2-pyridinecarboxamide is as follows: react 4.00g (23.8mmol) 5-nitropyridine-2-carboxylic acid with 1.91g (35.7mmol, 1.5 equivalents) ammonium chloride . After work-up, the crude product was used in the next stage without further purification. The 5-nitropyridine-2-carboxamide of the crude product (about 23.8 mmol) was reduced to obtain the 5-amino-2-pyridine carboxamide product, which was purified by normal phase chromatography (eluent: dichloromethane/ Methanol (9:1), containing 1.5% concentrated ammonia). Yield: 1.40 g (42% of theoretical value)
