反応 #92987

反応方程式

16β-ethyl-bromoacetoxy-4-estren-3-one

potassium isobutyrate

→

above-identified compound

収率 70.8%

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

収率 70.8%

溶媒

acetone

water

反応条件

後処理

1. 1
   温度the solution is refluxed for 6 hours
2. 2
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure
3. 3
   抽出the residue is extracted with 200 ml of ethyl acetate
4. 4
   その他The organic layer is separated
5. 5
   洗浄washed with water and saturated aqueous sodium chloride
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
8. 8
   洗浄passage of 100 ml of diisopropyl ether, elution
9. 9
   その他The eluate is evaporated under reduced pressure
10. 10
    その他to remove the solvent

実験手順

In a mixture of 50 ml of acetone and 10 ml of water are dissolved 1.5 g of 16β-ethyl-bromoacetoxy-4-estren-3-one and 0.8 g of potassium isobutyrate and the solution is refluxed for 6 hours. The acetone is distilled off under reduced pressure and the residue is extracted with 200 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride 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 100 ml of diisopropyl ether, elution is carried out with 300 ml of ethyl ether. The eluate is evaporated under reduced pressure to remove the solvent, giving 1.08 g of the above-identified compound as a viscous oil.

出典