反応 #63740

反応方程式

2,3,4-trimethylpyridine N-oxide

trichloroacetyl chloride

sodium bicarbonate

→

2-chloromethyl-3,4-dimethylpyridine

溶媒

chloroform

反応条件

後処理

1. 1
   温度at reflux under argon
2. 2
   workup.ADDITIONis added
3. 3
   抽出the mixture is extracted with methylene chloride
4. 4
   乾燥the methylene chloride solution is dried
5. 5
   濃縮concentrated
6. 6
   その他The thus-obtained crude product
7. 7
   その他is chromatographed on silica gel (solvent: methylene chloride/ether [5:1])

実験手順

A solution of 13.3 g of 2,3,4-trimethylpyridine N-oxide in 130 ml of abs. chloroform is boiled at reflux under argon and treated through the condenser with 33.2 ml of trichloroacetyl chloride. After 18 hours the reaction mixture is poured on to ice, whereupon 10% sodium bicarbonate solution is added, the mixture is extracted with methylene chloride and the methylene chloride solution is dried and concentrated. The thus-obtained crude product is chromatographed on silica gel (solvent: methylene chloride/ether [5:1]). The 2-chloromethyl-3,4-dimethylpyridine obtained is processed directly.

出典