反応 #710479

反応方程式

difluoroacetic acid

EDC-HCl

2-aminopyridine

→

2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide

収率 14.0%

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   洗浄washed once with water and twice with a 1% HCl aqueous solution
2. 2
   乾燥dried over anhydrous magnesium sulfate
3. 3
   濃縮concentrated under reduced pressure

実験手順

400 mg (4.26 mmol) of 2-aminopyridine was dissolved in 10 ml of anhydrous dichloromethane, 322 μl (490 mg, 5.11 mmol) of difluoroacetic acid, 982 mg (5.10 mmol) of EDC-HCl and 622 mg (5.11 mmol) of DMAP were added thereto, and the resulting mixture was stirred at room temperature for 61 hours. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed once with water and twice with a 1% HCl aqueous solution, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 102 mg (yield 14%) of 2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide.

出典