Reaktion #1865050

Reaktionsgleichung

4-fluoropyridin-2-amine

NIS

TFA

→

title compound

4-fluoro-5-iodopyridin-2-amine

Lösungsmittel

MeCN

EtOAc

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenwashed with sat. aq. Na2S2O3 (2×5 l), brine (4×5 l)
2. 2
   TrocknenThe combined organic layers were dried over Na2SO4
3. 3
   Filtrationfiltered
4. 4
   Einengenconcentrated
5. 5
   Sonstigeto get the crude product
6. 6
   SonstigeThe crude product was purified by recrystallization from EtOAc/pentane (1/10)

Vorschrift

A suspension of 4-fluoropyridin-2-amine (336 g, 2.5 mol) and NIS (745 g, 2.75 mol) in MeCN (9 l) was treated with TFA (114 g, 1 mol). The reaction mixture was then stirred at room temperature for 8 h. The reaction mixture was diluted with EtOAc (10 l), washed with sat. aq. Na2S2O3 (2×5 l), brine (4×5 l). The combined organic layers were dried over Na2SO4, filtered and concentrated to get the crude product. The crude product was purified by recrystallization from EtOAc/pentane (1/10) to afford the title compound as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 8.14 (d, 1H), 6.45 (s, 2H), 6.33 (d, 1H).

Quelle