Tri-o-tolylphosphine → 1-[2-Chloro-4-(trifluoromethyl)phenyl]piperazine

Temperatur

100 °C

A mixture of 0.5 g (1.6 mmol) of 3-chloro-4-iodobenzotrifluoride 0.7 g (3.8 mmol), N-Boc-piperazine, 41 mg (0.04 mmol) Tris(dibenzylideneacetone)dipalladium chloroform complex, 0.44 g (4.43 mmol) sodium-t-butoxide and 48 mg (0.16 mmol) tri-o-tolylphosphine in 6 ml dioxane was heated overnight at 100° C. The solution was allowed to cool to room temperature, taken up in ether (30 ml) and washed with brine (25 ml). The organic layer was dried over Na2SO4, filtered and the solvent was removed in vacuo. The crude oil was chromatographed over on silica gel: Eluent: Heptane-AcOEt 0-10% over 15 min to provide the title compound (0.06 g, 10%) as a brown oil, MS (m/e): 365.1 (MH+, 100%).

1. temperatureto cool to room temperature
2. washwashed with brine (25 ml)
3. dry with materialThe organic layer was dried over Na2SO4
4. filtrationfiltered
5. customthe solvent was removed in vacuo
6. customThe crude oil was chromatographed over on silica gel

ORD-Eintrag

ord-81443adcf32b432695227f565089dcc7

Quelldatensatz

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07427612B2