Isopropyl iodide → HCID 58356337, Verbindung

Temperatur

55 °C

A mixture of ethyl 2H-1,2,3-triazole-4-carboxylate (1.5 g), potassium carbonate (2.64 g) and 2-iodopropane (1.91 ml) in dry acetonitrile (30 ml) was stirred at 50-60° C. under nitrogen for 2 h. Further 2-iodopropane (0.955 ml) was added and the mixture was stirred at 50-60° C. under nitrogen for 1.5 h. The mixture was cooled to room temperature and allowed to stand for 4 days. The mixture was filtered through a 2 g silica SPE column eluting with ethyl acetate. The solution was concentrated in vacuo, Purification by chromatography on silica gel (100 g cartridge), eluting with a gradient of 0-100% ethyl acetate in cyclohexane over 40 min gave the title compound (315 mg) as a colourless oil.

1. stirringthe mixture was stirred at 50-60° C. under nitrogen for 1.5 h
2. temperatureThe mixture was cooled to room temperature
3. waitto stand for 4 days
4. filtrationThe mixture was filtered through a 2 g silica SPE column
5. washeluting with ethyl acetate
6. concentrationThe solution was concentrated in vacuo, Purification by chromatography on silica gel (100 g cartridge)
7. washeluting with a gradient of 0-100% ethyl acetate in cyclohexane over 40 min

ORD-Eintrag

ord-a84413b1b4a44e7bb564e137309053d9

Quelldatensatz

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08658635B2