反应详情

4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl methanesulfonate (436 mg), dissolved in abs. MeOH (7 ml), was added dropwise to a methanolic ammonia solution (7.1 ml; 7N) in a microwave vessel at RT and with stirring in the course of 10 min. After standing overnight, the solvent was stripped off and the residue was purified by means of preparative HPLC. The product-containing fractions were combined, freed from the acetonitrile and freeze-dried. The product was treated with saturated sodium chloride solution and rendered alkaline with potassium carbonate. After extraction with methylene chloride, the combined organic phases were dried with sodium sulfate, filtered and concentrated. 71 mg of the title compound were obtained.

1. waitAfter standing overnight
2. customthe residue was purified by means of preparative HPLC
3. customfreeze-dried
4. additionThe product was treated with saturated sodium chloride solution
5. extractionAfter extraction with methylene chloride
6. dry with materialthe combined organic phases were dried with sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated