تفاعل #93002

معادلة التفاعل

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

N,N-dimethylaniline

2-methylvaleryl chloride

→

above-identified compound

المردود 19.8%

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

المردود 19.8%

المذيبات

dichloromethane

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONis added to the above solution
2. 2
   درجة الحرارةThe mixture is refluxed for 6 hours
3. 3
   درجة الحرارةAfter cooling
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
6. 6
   غسيلpassage 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
   أخرىThe eluate is evaporated under reduced pressure
9. 9
   أخرىto remove the solvent

الإجراء التجريبي

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.

المصدر