Reaktion #50579

Reaktionsgleichung

α,α-bis(trifluoromethyl)-4,5-bis(4-fluorophenyl)-1-methyl-1H-imidazole-2-methanamine

cyclohexane carbonyl chloride

→

5-cyclohexyl-2,3-bis(4-fluorophenyl)-7,7-bis(trifluoromethyl)-7H-imidazo[1,5-A]-imidazole

Ausbeute 46.9%

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe mixture was purified by column chromatography
2. 2
   Wascheneluting with hexane
3. 3
   workup.ADDITIONmixture of hexane-ethylacetate (9:1)

Vorschrift

To a solution of α,α-bis(trifluoromethyl)-4,5-bis(4-fluorophenyl)-1-methyl-1H-imidazole-2-methanamine (3.38 gr, 7.8 mmole) in pyridine (1.7 gr) was added cyclohexane carbonyl chloride (3.5 gr, 23.9 mmole). The reaction mixture was heated at 130° C. for 4 hours. The mixture was purified by column chromatography, eluting with hexane, then mixture of hexane-ethylacetate (9:1) to give 5-cyclohexyl-2,3-bis(4-fluorophenyl)-7,7-bis(trifluoromethyl)-7H-imidazo[1,5-A]-imidazole (1.88 gr, 37%) as a white solid: mp 162.2-162.6. Anal. Calcd for C25H19F8N3 :C,58.60;H,3.54;N,8.20. Found: C,58.43;H,3.79;N,8.16.

Quelle