تفاعل #61830

ord-e7f5a3b6bf3c409fb2ace8e43952cc6f

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىprepared
  2. 2
    أخرىirradiation at 180° C.
  3. 3
    أخرىThe solvent was removed in vacuo
  4. 4
    أخرىthe residue was purified by silica gel chromatography
  5. 5
    غسيلeluting with 50% EtOAc/hexane

الإجراء التجريبي

A mixture of 2-chloro-5-(trifluoromethyl)-1H-benzo[d]imidazole (89 mg, 0.4 mol, prepared according to the procedure described in WO 2004/035549 A1), 5,6,7,8-tetrahydronaphthalene-1,7-diol from step (a) above (49 mg, 0.3 mmol) and 2-methoxy-ethanol (1 mL, Aldrich) was subjected to microwave irradiation at 180° C. with stirring for 60 min twice. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 50% EtOAc/hexane to give the title compound as an amorphous solid. MS (ESI, pos. ion) m/z: 349 (M+1).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07429608B2uspto-grants-2008_09