反应详情

A solution of 5-fluoro-2-nitrobenzoyl chloride (52 g, 0.256 mol) in a toluene (50 mL) and acetone (60 mL) mixture is added dropwise to a solution of sodium azide (19.55 g, 0.301 mol) in water while maintaining the reaction mixture temperature below 30° C. The resultant solid is collected and the filtrate is extracted with ether. The organic extracts are combined, washed with water, dried over anhydrous magnesium sulfate and concentrated by blowing air over the solution to obtain additional solids. The solids are combined, slurried in an acetone/water (1:3) solution, filtered and dried to give the title product as a yellow solid.

1. temperaturewhile maintaining the reaction mixture temperature below 30° C
2. customThe resultant solid is collected
3. extractionthe filtrate is extracted with ether
4. washwashed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. customto obtain additional solids
8. filtrationfiltered
9. customdried