反応 #1783

反応方程式

2-ethyl-3-chloromethylpyridine

m-chloroperbenzoic acid

→

2-ethyl-3-chloromethylpyridine-N-oxide

溶媒

CHCl3

反応条件

後処理

1. 1
   抽出The reaction was extracted twice with saturated aqueous sodium bicarbonate (100 mL)
2. 2
   乾燥The organic phase was dried with MgSO4
3. 3
   ろ過filtered
4. 4
   その他the solvent was removed under reduced pressure
5. 5
   その他The residue was chromatographed on silica gel
6. 6
   洗浄MeOH and eluted with the same
7. 7
   その他the solvent removed under reduced pressure the

実験手順

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.

出典