反応 #992707

反応方程式

2,6-Diaminopyridine

4-fluorobenzoyl chloride

→

2,6-bis(4-fluorobenzoylamino)pyridine

溶媒

dichloromethane

反応条件

後処理

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
   温度to warm to room temperature (25° C.)
4. 4
   workup.STIRRINGstirred for 18 hours
5. 5
   その他The resulting precipitate was isolated by filtration and suction
6. 6
   その他dried
7. 7
   その他The precipitate was recrystallized from 300 milliliters of refluxing ethanol
8. 8
   その他isolated by filtration
9. 9
   洗浄rinsed with ethanol, suction
10. 10
    その他dried
11. 11
    その他vacuum dried in an oven overnight

実験手順

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.

出典