Reaktion #675802

Reaktionsgleichung

ethyl 2-(5-acetamido-3-phenyl-pyrazol-1-yl)acetate

iodic acid

iodine

→

title compound

Ethyl 2-(5-acetamido-4-iodo-3-phenyl-pyrazol-1-yl)acetate

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled to room temperature
2. 2
   EinengenThe reaction mixture was concentrated in vacuo
3. 3
   workup.DISSOLUTIONthe residue was dissolved in CH2Cl2 (250 mL)
4. 4
   WaschenThe solution was washed twice with 2 M Na2S2O3
5. 5
   TrocknenThe organic layer was dried (magnesium sulphate)
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated in vacuo
8. 8
   SonstigeThe residue was triturated from diethyl ether
9. 9
   Filtrationfiltered
10. 10
    Sonstigedried

Vorschrift

A suspension of ethyl 2-(5-acetamido-3-phenyl-pyrazol-1-yl)acetate (34.81 g, 60.6 mmol), iodic acid (5.33 g, 30.3 mmol) and iodine (15.37 g, 60.6 mmol) in ethanol (250 mL) was heated at 50° C. for 1.5 h and cooled to room temperature. The reaction mixture was concentrated in vacuo and the residue was dissolved in CH2Cl2 (250 mL). 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 solid (44.13 g).

Quelle