反应详情

A solution of 183 mg of 2,3-dimethylpyridine 1-oxide in 0.6 ml of concentrated sulfuric acid was treated while cooling with ice with 0.2 ml of 65% nitric acid (d =1.4). The reaction mixture was stirred at 90° for 24 hours and poured on to a mixture of ice and sodium carbonate, whereupon the resulting mixture was extracted with methylene chloride and the methylene chloride phase was dried and evaporated. The residue, crystallized from ethanol/n-pentane, gave 2,3-dimethyl-4-nitropyridine 1-oxide of melting point 99-102°.

1. extractionwas extracted with methylene chloride
2. dry with materialthe methylene chloride phase was dried
3. customevaporated
4. customThe residue, crystallized from ethanol/n-pentane