반응 #78394

ord-99fa2889009c44f08cb79bded6f748b6

용매

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 9 h
  2. 2
    여과filtered
  3. 3
    농축The filtrate was concentrated to a volume of 30 ml under diminished pressure
  4. 4
    workup.ADDITIONafter addition of 150 ml of acetonitrile again to a volume
  5. 5
    여과the precipitated crystals were filtered
  6. 6
    세척washed twice with 25 ml of cold acetonitrile
  7. 7
    기타dried at 70° C.

실험 절차

In a 500 ml flask a mixture of 200 ml of dry ethanol, 20 g (0.026 mol) of 2-n-butyl-4-chloro-1-[(2′-(2-triphenylmethyl -2H-tetrazol-5-yl)-1,1′-biphenyl-4-yl)-methyl]1H-imidazol-5-methanol methyl-isobutyl ketone solvate and 1.45 g (0.026 mol) of potassium hydroxide was refluxed for 9 h, treated with 0.5 g of charcoal and filtered. The filtrate was concentrated to a volume of 30 ml under diminished pressure, and after addition of 150 ml of acetonitrile again to a volume: of 60 ml. The suspension was stirred at 0° C. for 1 h, the precipitated crystals were filtered, washed twice with 25 ml of cold acetonitrile and dried at 70° C. to give 10.6 g (88%) of the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06710183B2uspto-grants-2004_03