반응 #81727

반응 방정식

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

K2CO3

water

methanol

→

title compound

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

용매

ethyl acetate

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux overnight
3. 3
   농축The reaction mixture was then concentrated
4. 4
   workup.ADDITIONThe residue was diluted with water
5. 5
   추출extracted with ethyl acetate
6. 6
   추출The organic extract
7. 7
   세척was washed with brine
8. 8
   기타dried
9. 9
   농축concentrated
10. 10
    세척The resulting solid was washed with CH3CN
11. 11
    기타isolated by filtration
12. 12
    기타to give

실험 절차

A mixture of methyl-17β-cyclohexylcarbonyl-estra-1,3,5(10)-triene-3-carboxylate (0.14 g, 0.34 mmol), K2CO3 (0.2 g, 1.45 mmol), water (3.0 mL) and methanol (30 mL) was heated at reflux overnight. The reaction mixture was then concentrated. The residue was diluted with water, acidified with dilute HCl and extracted with ethyl acetate. The organic extract was washed with brine, dried, and concentrated. The resulting solid was washed with CH3CN and isolated by filtration from boiling ethyl acetate to give, 0. 11 g of the title compound. mp 280°-285° C. (softened at 260° C.).

출처