反应详情

Sodium azide (4.4 g, 68 mmol) was added to a suspension of 4-(4-bromo-2-chlorophenylamino)-5,6-dichloronicotinic acid methyl ester (26) (13.89 g, 33.8 mmol) in DMF (200 mL) and the mixture allowed to stir at room temperature overnight. The solution was diluted with water (600 mL) and the resulting white precipitate was collected by filtration and washed with water. The solids were dissolved into THF. Two volumes of diethyl ether were added and the organic solution washed with brine, dried over NaSO4, filtered, and concentrated in vacuo to the desired product (27) as a light yellow solid (12.94 g, 92%).

1. filtrationthe resulting white precipitate was collected by filtration
2. washwashed with water
3. dissolutionThe solids were dissolved into THF
4. additionTwo volumes of diethyl ether were added
5. washthe organic solution washed with brine
6. dry with materialdried over NaSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo to the desired product (27) as a light yellow solid (12.94 g, 92%)