Reaktion #992707

Reaktionsgleichung

2,6-Diaminopyridine

4-fluorobenzoyl chloride

→

2,6-bis(4-fluorobenzoylamino)pyridine

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

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
   Temperaturto warm to room temperature (25° C.)
4. 4
   workup.STIRRINGstirred for 18 hours
5. 5
   SonstigeThe resulting precipitate was isolated by filtration and suction
6. 6
   Sonstigedried
7. 7
   SonstigeThe precipitate was recrystallized from 300 milliliters of refluxing ethanol
8. 8
   Sonstigeisolated by filtration
9. 9
   Waschenrinsed with ethanol, suction
10. 10
    Sonstigedried
11. 11
    Sonstigevacuum dried in an oven overnight

Vorschrift

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.

Quelle