반응 #2286440

반응 방정식

2-chloro-3-fluoro-5-methylpyridine

N-bromosuccinimide

→

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

수율 51.0%

용매

carbon tetrachloride

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도under reflux overnight
3. 3
   기타After completion of the reaction
4. 4
   기타the reaction liquid
5. 5
   기타was returned to room temperature
6. 6
   농축concentrated under reduced pressure
7. 7
   기타Then, the residue was purified by silica gel column chromatography (hexane:ethyl acetate=19:1)

실험 절차

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%).

출처