반응 #92997

반응 방정식

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

monosodium succinate

→

above-identified compound

수율 24.5%

16β-Ethyl-17β-(2-carboxyethyl)carbonyloxyacetoxy-4-estren-3-one

수율 24.5%

용매

acetone

반응 조건

후처리

1. 1
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure
2. 2
   추출the residue is extracted with 150 ml of ethyl acetate
3. 3
   기타The organic layer is separated
4. 4
   세척washed with water and saturated aqueous sodium chloride solution
5. 5
   건조dried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
7. 7
   세척passage of 450 ml of chloroform, elution
8. 8
   기타The eluate is evaporated under reduced pressure
9. 9
   기타to remove the solvent
10. 10
    기타giving colorless crystals
11. 11
    세척The product is washed with petroleum ether
12. 12
    기타dried

실험 절차

In 100 ml of 50% aqueous acetone are dissolved 1.5 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 0.7 g of monosodium succinate and the solution is stirred at room temperature (15°-25° C.) for 3 days. The acetone is 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 solution and dried over anhydrous sodium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 450 ml of chloroform, elution is carried out with 150 ml of ethyl acetate. The eluate is evaporated under reduced pressure to remove the solvent, giving colorless crystals. The product is washed with petroleum ether and dried to give 0.4 g of the above-identified compound.

출처