반응 #1783

반응 방정식

2-ethyl-3-chloromethylpyridine

m-chloroperbenzoic acid

→

2-ethyl-3-chloromethylpyridine-N-oxide

용매

CHCl3

반응 조건

후처리

1. 1
   추출The reaction was extracted twice with saturated aqueous sodium bicarbonate (100 mL)
2. 2
   건조The organic phase was dried with MgSO4
3. 3
   여과filtered
4. 4
   기타the solvent was removed under reduced pressure
5. 5
   기타The residue was chromatographed on silica gel
6. 6
   세척MeOH and eluted with the same
7. 7
   기타the solvent removed under reduced pressure the

실험 절차

The 2-ethyl-3-chloromethylpyridine (2.4 g, 15.4 mmol) was dissolved in CHCl3 (100 mL) and cooled under nitrogen to 0° C. and m-chloroperbenzoic acid (55%, 4.2 g) was added in small portions. The reaction was stirred for 2 hours. The reaction was extracted twice with saturated aqueous sodium bicarbonate (100 mL). The organic phase was dried with MgSO4, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel packed in 98:2 CH2Cl2 :MeOH and eluted with the same. The appropriate fractions were combined and the solvent removed under reduced pressure the give the desired 2-ethyl-3-chloromethylpyridine-N-oxide.

출처