反応 #92986

反応方程式

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

potassium propionate

→

above-identified compound

収率 35.4%

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

収率 35.4%

溶媒

acetone

water

反応条件

後処理

1. 1
   濃縮concentrated under reduced pressure
2. 2
   抽出The residue is extracted with 200 ml of ethyl acetate
3. 3
   その他The organic layer is separated
4. 4
   洗浄washed with water and saturated aqueous sodium chloride
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
7. 7
   洗浄passage of 1000 ml isopropyl ether-n-hexane (2:3), elution
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 a mixture of 50 ml of acetone and 12 ml of water are dissolved 2.5 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one and 0.7 g of potassium propionate. The solution is stirred at room temperature (17°-25° C.) for 3 days and concentrated under reduced pressure. 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 distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 1000 ml isopropyl ether-n-hexane (2:3), elution is carried out with 2000 ml of the same solvent system. The eluate is evaporated under reduced pressure to remove the solvent, giving 0.87 g of the above-identified compound as white crystals.

出典