반응 #81724

반응 방정식

methyl 17β-benzoyl-estra-1,3,5(10)-triene-3-carboxylate

K2CO3

water

→

title compound

17β-Benzoyl-estra-1,3,5(10)-triene-3-carboxylic Acid

용매

methanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 5 h
3. 3
   기타The volatiles were then removed at reduced pressure
4. 4
   workup.ADDITIONthe residue was diluted with water
5. 5
   추출extracted with EtOAc
6. 6
   추출The organic extract
7. 7
   세척was washed with water and brine
8. 8
   기타dried
9. 9
   기타evaporated to dryness

실험 절차

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.

출처