Iodine → ethyl 2-(5-acetamido-4-iodo-3-phenyl-1H-pyrazol-1-yl)acetate
Reaktionsgleichung
[C:1]([NH:4][C:5]1[N:9]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:8]=[C:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:6]=1)(=[O:3])[CH3:2].[I:22](O)(=O)=O.II>C(O)C>[C:1]([NH:4][C:5]1[N:9]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:8]=[C:7]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:6]=1[I:22])(=[O:3])[CH3:2]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
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).
Aufarbeitung
- temperaturecooled to room temperature
- concentrationThe reaction mixture was concentrated in vacuo
- dissolutionthe residue was dissolved in CH2Cl2 (250 mL)
- washThe solution was washed twice with 2 M Na2S2O3
- dry with materialThe organic layer was dried (magnesium sulphate)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue was triturated from diethyl ether
- filtrationfiltered
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-87b9eef60b0f4b99a98579326a5a4263
- Quelldatensatz
- uspto-grants-2016_06
- Patentnummer
- US09371332B2
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