反应详情

A solution of phosphoryl chloride (6.5 g) in dichloromethane (20 ml) was added to a mixture of the above pyridine-1-oxide (4.4 g) and triethylamine (4.3 g) in dichloromethane (60 ml). After the addition was completed the reaction mixture was gently refluxed for 15 mins, cooled and washed with water (30 ml). The organic layer was separated, dried over anhydrous sodium sulphate and evaporated to dryness. The residue was purified by flash column chromatography on silica (K60) using ethyl acetate: toluene (1:9 by volume) as eluting solvent, to give 6-chloromethylnicotinonitrile.

1. additionAfter the addition
2. temperaturewas gently refluxed for 15 mins
3. temperaturecooled
4. washwashed with water (30 ml)
5. customThe organic layer was separated
6. dry with materialdried over anhydrous sodium sulphate
7. customevaporated to dryness
8. customThe residue was purified by flash column chromatography on silica (K60)
9. washas eluting solvent