反应详情

To 4-[4-(methylamino)-3-nitrophenoxy]pyridine carboxylic acid in tetrahydro-furan was added EDC (2 eq) and HOAT (1.5 eq) and ammonium chloride (2 eq). The resulting mixture was stirred at ambient temperature for 16 h. The mixture was concentrated and partitioned between ethylacetate and water. A solid crashes out in the aqueous layer which was filtered and was found to be the product on LC/MS. The organic layer was then dried with sodium sulfate and concentrated. Purification on silica gel gave 4-[4-(methylamino)-3-nitrophenoxy]pyridine-2-carboxamide.

1. concentrationThe mixture was concentrated
2. custompartitioned between ethylacetate and water
3. filtrationA solid crashes out in the aqueous layer which was filtered
4. dry with materialThe organic layer was then dried with sodium sulfate
5. concentrationconcentrated
6. customPurification on silica gel