反应详情

Benzyl carbazate (27.8 g), 1-hydroxybenztriazole (24.8 g) and 1-ethyl-3-(dimethylaminopropyl)carbodiimide hydrochloride (35.4 g) were sequentially added to a solution of 6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridine-2-carboxylic acid obtained in Preparation Example 1-5 (51.9 g) and IPEA (44 mL) in N,N-dimethylformamide (184 mL), and the mixture was stirred at room temperature for six hours and 30 minutes. Ethyl acetate, ice water and a saturated sodium bicarbonate solution were added to the reaction solution, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and then filtered through an NH silica gel pad. The resulting filtrate was concentrated under reduced pressure. Ethyl acetate was added to the resulting residue, and the powder was collected by filtration. The resulting powder was air-dried to obtain 28.4 g of the title compound.

1. customthe organic layer was separated
2. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
3. filtrationfiltered through an NH silica gel pad
4. concentrationThe resulting filtrate was concentrated under reduced pressure
5. additionEthyl acetate was added to the resulting residue
6. filtrationthe powder was collected by filtration
7. customThe resulting powder was air-dried