反応 #62343

反応方程式

2-amino-4-methyl-5-nitropyridine

isopentyl sulfite

diiodomethane

→

title compound

2-Iodo-4-methyl-5-nitropyridine

反応条件

後処理

1. 1
   workup.STIRRINGthe solution was stirred for 2 hours
2. 2
   その他The diiodomethane was evaporated
3. 3
   その他the crude product was purified
4. 4
   その他separated by silica gel column chromatography (ethyl acetate:n-hexane=1:20)

実験手順

To a solution of 1.0 g of 2-amino-4-methyl-5-nitropyridine in 10 mL of diiodomethane was added 1.8 mL of isopentyl sulfite at room temperature, stirred at this temperature for 30 minutes, and after raising the temperature to 80° C., the solution was stirred for 2 hours. The diiodomethane was evaporated, and the crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:20), to afford 897 mg of the title compound as colorless crystals.

出典