Triphosgene → HCID 86625045, Verbindung

Temperatur

100 °C

5-Chloro-2-iodo-4-(trifluoromethyl)aniline D10 (7.7 mmol, 2.2 g), bis(trichloromethyl) carbonate (0.35 eq., 2.7 mmol, 800 mg) were dissolved in 1,4-dioxane (10 ml) and the mixture was heated to 100° C. for 15 minutes; the mixture was then cooled to room temperature and it was filtered. The filtrate was concentrated to afford 1-chloro-4-iodo-5-isocyanato-2-(trifluoromethyl)benzene which was dissolved in dichloromethane (10 ml) and 1,1-dimethylethyl 4-amino-1-piperidinecarboxylate (2 eq., 11.4 mmol, 2.28 g) was added at room temperature; the mixture was stirred at room temperature for 1.5 hours. Solvent was subsequently evaporated and the crude obtained was purified by chromatography (ethyl acetate-n-hexane) to afford the title compound, 1.46 g, 46%, M+−H=546.

1. temperaturethe mixture was then cooled to room temperature
2. filtrationit was filtered
3. concentrationThe filtrate was concentrated

ORD-Eintrag

ord-50dce8242d7f41bc8da20d0c2e6c4ae6

Quelldatensatz

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08288412B2