تفاعل #76531

ord-0d28696821f74aee8587ed8722bf4a8d

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITto proceed for eighteen hours at room temperature
  2. 2
    تركيزit was concentrated to dryness in vacuo
  3. 3
    workup.ADDITION500 mL of EtOAc was slowly added along with 2 mL of water
  4. 4
    workup.STIRRINGAfter stirring for 10 minutes
  5. 5
    workup.ADDITION500 mL of water was added
  6. 6
    أخرىthe EtOAc layer was removed
  7. 7
    غسيلThe EtOAc layer was washed with an additional 500 mL of water
  8. 8
    أخرىthe layers were separated
  9. 9
    تجفيفThe EtOAc layer was dried with anhydrous Na2SO4
  10. 10
    تركيزconcentrated to dryness

الإجراء التجريبي

4.57 g (0.01 mol) of [2-(4-hydroxyphenyl)-6-hydroxybenzofuran-3-yl][4-[2-(1-piperidinyl)ethoxy]phenyl] methanone was dissolved in 250 mL of THF and 2 g (0.053 mol) of LiAlH4 was slowly added over a period of twenty minutes to the stirring solution. The reaction mixture was stirred and kept under a nitrogen atmosphere and the reaction was allowed to proceed for eighteen hours at room temperature and then it was concentrated to dryness in vacuo. 500 mL of EtOAc was slowly added along with 2 mL of water. After stirring for 10 minutes, 500 mL of water was added and the EtOAc layer was removed. The EtOAc layer was washed with an additional 500 mL of water and the layers were separated. The EtOAc layer was dried with anhydrous Na2SO4 and concentrated to dryness to yield 2.66 g of the title compound as tan amorphous powder.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06703407B1uspto-grants-2004_03