반응 #93002

반응 방정식

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

N,N-dimethylaniline

2-methylvaleryl chloride

→

above-identified compound

수율 19.8%

16β-Ethyl-17β-(2-methylvaleryl)oxyacetoxy-4-estren-3-one

수율 19.8%

용매

dichloromethane

ethyl acetate

반응 조건

후처리

1. 1
   workup.ADDITIONis added to the above solution
2. 2
   온도The mixture is refluxed for 6 hours
3. 3
   온도After cooling
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
6. 6
   세척passage of 200 ml of diisopropyl ether-n-hexane (2:8), elution
7. 7
   workup.ADDITIONis carried out with 500 ml of a 1:1 mixture of the same solvents
8. 8
   기타The eluate is evaporated under reduced pressure
9. 9
   기타to remove the solvent

실험 절차

In 20 ml of dichloromethane are dissolved 0.5 g of 16β-ethyl-17β-glycoloyloxy-4-estren-3-one and 0.2 ml of N,N-dimethylaniline, and 0.5 g of 2-methylvaleryl chloride is added to the above solution. The mixture is refluxed for 6 hours. After cooling, the reaction mixture is diluted with 150 ml of ethyl acetate and dried over anhydrous magnesium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 200 ml of diisopropyl ether-n-hexane (2:8), elution is carried out with 500 ml of a 1:1 mixture of the same solvents. The eluate is evaporated under reduced pressure to remove the solvent, giving 0.126 g of the above-identified compound as a light-yellow viscous oil.

출처