反応 #93002

反応方程式

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

N,N-dimethylaniline

2-methylvaleryl chloride

→

above-identified compound

収率 19.8%

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

収率 19.8%

溶媒

dichloromethane

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONis added to the above solution
2. 2
   温度The mixture is refluxed for 6 hours
3. 3
   温度After cooling
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
6. 6
   洗浄passage 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
   その他The eluate is evaporated under reduced pressure
9. 9
   その他to remove the solvent

実験手順

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.

出典