반응 #63737

반응 방정식

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

trichloroacetyl chloride

sodium bicarbonate

→

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

용매

chloroform

반응 조건

후처리

1. 1
   온도at reflux under argon
2. 2
   workup.ADDITIONis added
3. 3
   추출the mixture is extracted with methylene chloride
4. 4
   건조the methylene chloride solution is dried
5. 5
   농축concentrated
6. 6
   기타The thus-obtained crude product
7. 7
   기타is chromatographed on silica gel (solvent: methylene chloride/ether [10:1])

실험 절차

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.

출처