反応 #81724

反応方程式

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

溶媒

methanol

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux for 5 h
3. 3
   その他The volatiles were then removed at reduced pressure
4. 4
   workup.ADDITIONthe residue was diluted with water
5. 5
   抽出extracted with EtOAc
6. 6
   抽出The organic extract
7. 7
   洗浄was washed with water and brine
8. 8
   その他dried
9. 9
   その他evaporated to dryness

実験手順

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.

出典