反応 #63737

反応方程式

4-tert-butyl-2,3-dimethylpyridine N-oxide

trichloroacetyl chloride

sodium bicarbonate

→

2-chloromethyl-4-tert-butyl-3-methylpyridine

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 [10:1])

実験手順

A solution of 9.8 g of 4-tert-butyl-2,3-dimethylpyridine N-oxide in 120 ml of abs. chloroform is boiled at reflux under argon and treated through the condenser with 25.5 ml of trichloroacetyl chloride. After 22 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 [10:1]). The 2-chloromethyl-4-tert-butyl-3-methylpyridine obtained is processed directly.

出典