Iodine → HCID 178432833, Verbindung

Temperatur

60 °C

To 2-methyl-4-(trifluoromethyl)-1H-imidazole (1 g, 6.7 mmol) was added CHCl3 (4.5 mL) and AcOH (13.5 mL) followed by I2 (1.78 g, 6.99 mmol) and HIO4.2H2O (1.52 g, 6.7 mmol), and the resulting reaction mixture was stirred at 60° C. for 3 h. The reaction mixture was then poured into ice cold 10% aqueous sodium bisulphite solution (100 mL) and the aqueous layer was extracted with EtOAc (3×100 mL). The combined organic layers were washed with brine (100 mL), dried (MgSO4) and concentrated in vacuo to obtain 5-iodo-2-methyl-4-(trifluoromethyl)-1H-imidazole (1.98 g) which was used as such in next step without further purification.

1. customthe resulting reaction mixture
2. extractionthe aqueous layer was extracted with EtOAc (3×100 mL)
3. washThe combined organic layers were washed with brine (100 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo

ORD-Eintrag

ord-b79a78fc6cc248c9a7bf201f7e8a7dc8

Quelldatensatz

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09169248B2