تفاعل #92994

معادلة التفاعل

16β-ethyl-17β-bromoacetoxy-4-estren-3-one

sodium stearate

→

above-identified compound

المردود 57.1%

16β-Ethyl-17β-stearoyloxyacetoxy-4-estren-3-one

المردود 57.1%

المذيبات

acetone water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture is refluxed for 4 hours
2. 2
   أخرىto stand at room temperature
3. 3
   أخرى(15°-25° C.) overnight
4. 4
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
5. 5
   استخلاصthe residue is extracted with 150 ml of ethyl acetate
6. 6
   أخرىThe organic layer is separated
7. 7
   غسيلwashed with water and saturated aqueous sodium chloride
8. 8
   تجفيفdried over anhydrous sodium sulfate
9. 9
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
10. 10
    workup.DISSOLUTIONthe residue is dissolved in 100 ml of ethanol
11. 11
    workup.ADDITIONTo the solution is added 0.3 g of activated carbon
12. 12
    ترشيحthe insoluble material is filtered off
13. 13
    workup.DISTILLATIONThe solvent is distilled off
14. 14
    أخرىto give a colorless viscous oil, which
15. 15
    أخرىto stand at room temperature
16. 16
    أخرى(15°-25° C.)

الإجراء التجريبي

To 150 ml of acetone-water (2:1) are added 1.3 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 1.0 g of sodium stearate and the mixture is refluxed for 4 hours and allowed to stand at room temperature (15°-25° C.) overnight. The solvent is then distilled off under reduced pressure and the residue is extracted with 150 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride and dried over anhydrous sodium sulfate. The solvent is distilled off under reduced pressure and the residue is dissolved in 100 ml of ethanol. To the solution is added 0.3 g of activated carbon and the insoluble material is filtered off. The solvent is distilled off to give a colorless viscous oil, which is allowed to stand at room temperature (15°-25° C.) to give 1.1 g of the above-identified compound as a solid.

المصدر