Reaktion #974907

Reaktionsgleichung

N-iodosuccinimide

5-Amino-2-chloropyridine

Water

ether

→

title compound

Ausbeute 80.8%

3-amino-6-chloro-2-iodopyridine

Ausbeute 80.8%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe layers were separated
2. 2
   Waschenthe organic layer was washed 3× with water
3. 3
   Waschenwashed with brine
4. 4
   Trocknendried over MgSO4
5. 5
   Einengenconcentrated in vacuum
6. 6
   SonstigeThe residue was purified by column chromatography (silica 60, hexane/ethyl acetate=3:1, Rf=0.30)

Vorschrift

5-Amino-2-chloropyridine (3.0 g) was dissolved in DMF (40 mL), N-iodosuccinimide (5.25 g) was added and the reaction mixture was stirred at room temperature for 3 hours. Water and MTB-ether were added to the reaction mixture, the layers were separated and the organic layer was washed 3× with water, washed with brine, dried over MgSO4 and concentrated in vacuum. The residue was purified by column chromatography (silica 60, hexane/ethyl acetate=3:1, Rf=0.30) to afford 4.80 g of the title compound of the formula

Quelle