تفاعل #81724

ord-310ecfb86a4b40d589cf751e84ec977e

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux for 5 h
  3. 3
    أخرىThe volatiles were then removed at reduced pressure
  4. 4
    workup.ADDITIONthe residue was diluted with water
  5. 5
    استخلاصextracted with EtOAc
  6. 6
    استخلاصThe organic extract
  7. 7
    غسيلwas washed with water and brine
  8. 8
    أخرىdried
  9. 9
    أخرىevaporated to dryness

الإجراء التجريبي

A mixture of methyl 17β-benzoyl-estra-1,3,5(10)-triene-3-carboxylate (60 mg, 0.15 mmol), K2CO3 (60 mg, 0.44 mmol), water (1 mL), and methanol (9 mL) was heated at reflux for 5 h. The volatiles were then removed at reduced pressure and the residue was diluted with water, acidified with dilute aqueous HCl, and extracted with EtOAc. The organic extract was washed with water and brine, dried, and evaporated to dryness. Trituration of the residue with acetone and methanol provided the title compound as a white solid, mp 240°-243° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05618806uspto-grants-1997_04