Reaktion #675755

Reaktionsgleichung

N-(3-methyl-1H-pyrazol-5-yl)acetamide

iodic acid

iodine

→

title compound

N-(4-iodo-3-methyl-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
   WaschenThe solution was washed twice with 2 M Na2S2O3
4. 4
   TrocknenThe organic layer was dried (magnesium sulphate)
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated in vacuo
7. 7
   SonstigeThe residue was triturated from diethyl ether
8. 8
   Filtrationfiltered
9. 9
   Sonstigedried

Vorschrift

A suspension of N-(3-methyl-1H-pyrazol-5-yl)acetamide (29.6 g, 0.213 mol), iodic acid (9.3 g, 0.053 mol) and iodine (32.5 g, 0.128 mol) in ethanol (300 mL) was heated at 50° C. for 3 h and cooled to room temperature. The reaction mixture was concentrated in vacuo and taken up in ethyl acetate. The solution was washed twice with 2 M Na2S2O3 followed by brine solution. The organic layer was dried (magnesium sulphate), filtered and concentrated in vacuo. The residue was triturated from diethyl ether, filtered and dried to provide the title compound as a white solid (32.5 g).

Quelle