تفاعل #59785

ord-f9887d6df49a4def8df6b1b0afd0b0d4

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىNitrogen gas was bubbled through the reaction mixture
  2. 2
    أخرىto remove excess phosgene
  3. 3
    تركيزThe reaction mixture was concentrated to dryness
  4. 4
    أخرىthe residue was dried in vacuo for 1 h

الإجراء التجريبي

To a solution of 4,5-bis-(4-chloro-phenyl)-2-(2-ethoxy-4-trifluoromethyl-phenyl)-4,5-dihydro-1H-imidazole (46 g, 95.97 mmol, example 1) and triethylamine (66.9 mL, 479.9 mmol) in methylene chloride (2 L) cooled to 0° C. was added phosgene (124.3 mL, 239.9 mmol, ˜20% solution in toluene) dropwise over a period of 30 min. The reaction mixture was stirred at room temperature for 1 h. Nitrogen gas was bubbled through the reaction mixture to remove excess phosgene. The reaction mixture was concentrated to dryness, and the residue was dried in vacuo for 1 h to give 4,5-bis-(4-chloro-phenyl)-2-(2-ethoxy-4-trifluoromethyl-phenyl)-4,5-dihydro-imidazole-1-carbonyl chloride (51 g, 98% yield) as off-white solids. The product was used without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425638B2uspto-grants-2008_09