تفاعل #653190

ord-cc72d8134edc4aa2b1c1d5655a7a18ad

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزconcentrated under reduced pressure
  2. 2
    workup.ADDITIONTo the residue was added 1N hydrochloric acid (5 ml)
  3. 3
    استخلاصthe mixture was extracted with ethyl acetate
  4. 4
    غسيلThe organic layer was washed with saturated sodium chloride solution
  5. 5
    تجفيفdried with magnesium sulfate
  6. 6
    تركيزconcentrated
  7. 7
    ترشيحThe resulting crystal was collected by filtration

الإجراء التجريبي

To a solution of ethyl 7-(4-trifluoromethylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate (440 mg) in tetrahydrofuran-ethanol (10-10 ml) was added 1N sodium hydroxide (4.0 ml) at room temperature, and the mixture was stirred for 20 hours and concentrated under reduced pressure. To the residue was added 1N hydrochloric acid (5 ml), and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with magnesium sulfate and concentrated. The resulting crystal was collected by filtration to give 7-(4-trifluoromethylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (392 mg) as colorless crystals.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06172061B2uspto-grants-2001_01