تفاعل #2198044

ord-e521ddfe5258452abea2008398da02aa

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe mixture was stirred at the same temperature for 2.5 hr
  2. 2
    workup.ADDITIONwas added to the reaction mixture
  3. 3
    workup.STIRRINGthe mixture was stirred at room temperature for 2 hr
  4. 4
    ترشيحThe insoluble material was filtered off
  5. 5
    تركيزthe filtrate was concentrated under reduced pressure
  6. 6
    أخرىThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1-hexane/ethyl acetate=1/1)

الإجراء التجريبي

To a solution of methyl 4-[(3,5-diphenyl-1H-pyrazol-1-yl)methyl]-3-isopropoxybenzoate (0.59 g, 1.38 mmol) in tetrahydrofuran (12 mL) was added lithium aluminum hydride (52 mg, 1.38 mmol) with stirring at 0° C., and the mixture was stirred at the same temperature for 2.5 hr. After completion of the reaction, sodium sulfate decahydrate (0.89 g, 2.76 mmol) was added to the reaction mixture, and the mixture was stirred at room temperature for 2 hr. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=5/1-hexane/ethyl acetate=1/1) to give the title compound (0.50 g, yield 92%) as a colorless oil. MS (ESI+): 399 (M+H).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07517910B2uspto-grants-2009_04