反応 #81727

反応方程式

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

溶媒

ethyl acetate

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux overnight
3. 3
   濃縮The reaction mixture was then concentrated
4. 4
   workup.ADDITIONThe residue was diluted with water
5. 5
   抽出extracted with ethyl acetate
6. 6
   抽出The organic extract
7. 7
   洗浄was washed with brine
8. 8
   その他dried
9. 9
   濃縮concentrated
10. 10
    洗浄The resulting solid was washed with CH3CN
11. 11
    その他isolated by filtration
12. 12
    その他to give

実験手順

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.).

出典