반응 #78395

ord-d9115b6c6ab3431389654d5cc1bdafe8

용매

반응 조건

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

후처리

  1. 1
    온도was refluxed for 3 h
  2. 2
    여과filtered at room temperature
  3. 3
    농축The filtrate was concentrated to a volume of 30 ml under diminished pressure
  4. 4
    workup.ADDITIONafter addition of 160 ml of heptane again to a volume of 130 ml
  5. 5
    여과the precipitated crystals were filtered
  6. 6
    세척washed with cold heptane
  7. 7
    기타dried at 70° C.

실험 절차

Under nitrogen, in a 500 ml flask a mixture of 200 ml of dry methanol, 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 3 h, treated with 0.4 g of charcoal and filtered at room temperature. The filtrate was concentrated to a volume of 30 ml under diminished pressure, and after addition of 160 ml of heptane again to a volume of 130 ml. The suspension was stirred at 0° C. for 2 h, the precipitated crystals were filtered, washed with cold heptane and dried at 70° C. to give 11.3 g (92.5%) of the title compound.

출처

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