Реакция #92986

Уравнение реакции

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

potassium propionate

→

above-identified compound

Выход 35.4%

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

Выход 35.4%

Растворители

acetone

water

Условия реакции

Обработка

1. 1
   Концентрированиеconcentrated under reduced pressure
2. 2
   ЭкстракцияThe residue is extracted with 200 ml of ethyl acetate
3. 3
   ДругоеThe organic layer is separated
4. 4
   Промывкаwashed with water and saturated aqueous sodium chloride
5. 5
   Сушкаdried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
7. 7
   Промывкаpassage of 1000 ml isopropyl ether-n-hexane (2:3), elution
8. 8
   ДругоеThe eluate is evaporated under reduced pressure
9. 9
   Другоеto remove the solvent

Методика

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.

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