Реакция #992707

Уравнение реакции

2,6-Diaminopyridine

4-fluorobenzoyl chloride

→

2,6-bis(4-fluorobenzoylamino)pyridine

Растворители

dichloromethane

Условия реакции

Обработка

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
   Температураto warm to room temperature (25° C.)
4. 4
   workup.STIRRINGstirred for 18 hours
5. 5
   ДругоеThe resulting precipitate was isolated by filtration and suction
6. 6
   Другоеdried
7. 7
   ДругоеThe precipitate was recrystallized from 300 milliliters of refluxing ethanol
8. 8
   Другоеisolated by filtration
9. 9
   Промывкаrinsed with ethanol, suction
10. 10
    Другоеdried
11. 11
    Другоеvacuum dried in an oven overnight

Методика

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.

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