反应详情

Hydrogenate 13β-ethyl-3-acetoxygona-1,3,5(10),8,14-pentaen-17-one (1.8 g.) dissolved in benzene (25 ml.) at atmospheric pressure in the presence of 10% palladized charcoal (100 mg.). After 1.1 molar equivalents of hydrogen has been absorbed (ca. 12 hr.) filter off the catalyst, evaporate the filtrate under reduced pressure and recrystallize the residue from ethanol. Filter the red product through `Florisil` (60 g.) with benzene-petroleum (3:1), remove the solvent and recrystallize the product from ethanol to obtain the title product, m.p. 132.5°-134.5°; ultra-violet absorption peak at 277 mμ (ε 12,800).

1. customAfter 1.1 molar equivalents of hydrogen has been absorbed (ca. 12 hr.)
2. filtrationfilter off the catalyst
3. customevaporate the filtrate under reduced pressure
4. customrecrystallize the residue from ethanol
5. filtrationFilter the red product through `Florisil` (60 g.) with benzene-petroleum (3:1)
6. customremove the solvent
7. customrecrystallize the product from ethanol