تفاعل #544028

ord-306b11e3c58b49099bbfcf2a0da3500b

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed under nitrogen for 7 h
  2. 2
    ترشيحThe reaction was filtered
  3. 3
    workup.ADDITIONacidified by the addition of 2.5 mL of 1 N HCl
  4. 4
    تركيزconcentrated under reduced pressure
  5. 5
    أخرىto remove the THF and methanol
  6. 6
    ترشيحThe solid present was collected by filtration
  7. 7
    غسيلrinsed with water
  8. 8
    أخرىdried under reduced pressure

الإجراء التجريبي

A mixture of methyl 4-({[6-(1,5-diphenyl-1H-pyrrol-2-yl)-2-naphthyl]oxy}methyl)benzoate (235 mg, 0.461 mmol), prepared in the previous step, and 1 N NaOH (692 μL, 0.692 mmol) in 30 mL of THF plus 30 mL of methanol plus 5 mL of water was refluxed under nitrogen for 7 h. The reaction was filtered, cooled to room temperature, acidified by the addition of 2.5 mL of 1 N HCl and then concentrated under reduced pressure to remove the THF and methanol. The solid present was collected by filtration, rinsed with water and dried under reduced pressure to give the title compound (225 mg, 99%) as a white solid, mp 309–310° C. Elemental Analysis for C34H25NO3.0.05 C4H8O.0.19 H2O Calc'd: C, 81.73; H, 5.17; N, 2.79. Found: C, 81.94; H, 5.02; N, 2.65.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07186749B2uspto-grants-2007_03