반응 #5302

반응 방정식

sodium hydride

2-chloro-4-(3-bromophenoxy)phenol

2-chloro-5-chloromethylpyridine

→

2-chloro-5-[4-(3-bromophenoxy)-2-chlorophenoxy]methylpyridine

용매

N,N-dimethylformamide

N,N-dimethylformamide

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도ice-cooling
2. 2
   workup.WAITby stirrring at the same temperature for 10 hours
3. 3
   추출extracted twice with 100 ml of ethyl acetate
4. 4
   세척washed with water
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   농축concentrated under reduced pressure

실험 절차

To a solution of 0.07 g of sodium hydride (60% oil dispersion) in 10 ml of N,N-dimethylformamide, there is added dropwise a solution of 0.50 g of 2-chloro-4-(3-bromophenoxy)phenol in 3 ml of N,N-dimethylformamide with stirring and ice-cooling. After 30 minutes, a solution of 0.27 g of 2-chloro-5-chloromethylpyridine in 5 ml of N,N-dimethylformamide is added thereto at room tempearture, followed by stirrring at the same temperature for 10 hours. The reaction mixture is poured into ice-water and extracted twice with 100 ml of ethyl acetate. The extracts are combined together, washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue is subjected to silica gel chromatography to give 2-chloro-5-[4-(3-bromophenoxy)-2-chlorophenoxy]methylpyridine.

출처