Reacción #992707

Ecuación de reacción

2,6-Diaminopyridine

4-fluorobenzoyl chloride

→

2,6-bis(4-fluorobenzoylamino)pyridine

Disolventes

dichloromethane

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONtrietbylamine (28.0 milliliters, 20.2 grams, 0.2 mole) was added
2. 2
   workup.ADDITIONwas added drop-wise over the course of 30 minutes
3. 3
   Temperaturato warm to room temperature (25° C.)
4. 4
   workup.STIRRINGstirred for 18 hours
5. 5
   OtroThe resulting precipitate was isolated by filtration and suction
6. 6
   Otrodried
7. 7
   OtroThe precipitate was recrystallized from 300 milliliters of refluxing ethanol
8. 8
   Otroisolated by filtration
9. 9
   Lavadorinsed with ethanol, suction
10. 10
    Otrodried
11. 11
    Otrovacuum dried in an oven overnight

Procedimiento

2,6-Diaminopyridine (10.9 grams, 0.1 mole) was dissolved in 500 milliliters dichloromethane and trietbylamine (28.0 milliliters, 20.2 grams, 0.2 mole) was added. The solution was chilled to 0° C. before 4-fluorobenzoyl chloride (24.0 milliliters, 31.7 grams, 0.2 mole) was added drop-wise over the course of 30 minutes. After stirring for 2 hours at 0° C., the solution was allowed to warm to room temperature (25° C.) and stirred for 18 hours. The resulting precipitate was isolated by filtration and suction dried. The precipitate was recrystallized from 300 milliliters of refluxing ethanol, isolated by filtration, rinsed with ethanol, suction dried, and vacuum dried in an oven overnight. The yield was 34.0 grams of white crystals.

Fuente