تفاعل #81727

معادلة التفاعل

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

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةat reflux overnight
3. 3
   تركيزThe reaction mixture was then concentrated
4. 4
   workup.ADDITIONThe residue was diluted with water
5. 5
   استخلاصextracted with ethyl acetate
6. 6
   استخلاصThe organic extract
7. 7
   غسيلwas washed with brine
8. 8
   أخرىdried
9. 9
   تركيزconcentrated
10. 10
    غسيلThe resulting solid was washed with CH3CN
11. 11
    أخرىisolated by filtration
12. 12
    أخرىto give

الإجراء التجريبي

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.).

المصدر