Réaction #992707

Équation de réaction

2,6-Diaminopyridine

4-fluorobenzoyl chloride

→

2,6-bis(4-fluorobenzoylamino)pyridine

Solvants

dichloromethane

Conditions de réaction

Traitement

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
   Températureto warm to room temperature (25° C.)
4. 4
   workup.STIRRINGstirred for 18 hours
5. 5
   AutreThe resulting precipitate was isolated by filtration and suction
6. 6
   Autredried
7. 7
   AutreThe precipitate was recrystallized from 300 milliliters of refluxing ethanol
8. 8
   Autreisolated by filtration
9. 9
   Lavagerinsed with ethanol, suction
10. 10
    Autredried
11. 11
    Autrevacuum dried in an oven overnight

Mode opératoire

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.

Source