反応 #2286440

反応方程式

2-chloro-3-fluoro-5-methylpyridine

N-bromosuccinimide

→

5-(bromomethyl)-2-chloro-3-fluoropyridine

収率 51.0%

溶媒

carbon tetrachloride

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度under reflux overnight
3. 3
   その他After completion of the reaction
4. 4
   その他the reaction liquid
5. 5
   その他was returned to room temperature
6. 6
   濃縮concentrated under reduced pressure
7. 7
   その他Then, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=19:1)

実験手順

In 80 ml of carbon tetrachloride, 4.00 g (27.6 mmol) of 2-chloro-3-fluoro-5-methylpyridine was dissolved. To this solution, 7.37 g (41.4 mmol) of N-bromosuccinimide and 20 mg of benzoyl peroxide were added, and the mixture was heated under reflux overnight. After completion of the reaction, the reaction liquid was returned to room temperature, and concentrated under reduced pressure. Then, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=19:1). Thus, 3.06 g of 5-(bromomethyl)-2-chloro-3-fluoropyridine was obtained (Percentage Yield: 51%).

出典