Reaktion #675740

Reaktionsgleichung

N-(1H-pyrazol-5-yl)acetamide

iodic acid

iodine

→

title compound

N-(4-iodo-1H-pyrazol-5-yl)acetamide

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled to room temperature
2. 2
   EinengenThe reaction mixture was concentrated in vacuo
3. 3
   Sonstigepartitioned between ethyl acetate and 2 M Na2S2O3 aq. solution
4. 4
   SonstigeThe layers were separated
5. 5
   Extraktionthe aqueous extracted with ethyl acetate
6. 6
   TrocknenThe combined organic layers were dried (MgSO4)
7. 7
   Filtrationfiltered
8. 8
   Einengenconcentrated in vacuo

Vorschrift

A suspension of N-(1H-pyrazol-5-yl)acetamide (60 g, 0.48 mol), iodic acid (21.1 g, 0.12 mol) and iodine (61 g, 0.24 mol) in ethanol (1.6 L) was heated at 60° C. for 1.5 h and cooled to room temperature. The reaction mixture was concentrated in vacuo and partitioned between ethyl acetate and 2 M Na2S2O3 aq. solution. The layers were separated and the aqueous extracted with ethyl acetate. The combined organic layers were dried (MgSO4), filtered and concentrated in vacuo to provide the title compound as a solid (105 g).

Quelle