摘要 |
<p>Steroids I Intermediates for aldosterone and analogues. (a) To DELTA5-3:3:20:20-bisethylenedioxy-11beta:18-oxido-18-hydroxy-preg- nene (433 mg) in PhMei(40 ml) at 0-3 deg.C under N2, was added (5 min.) M-Bu2AlH in PhMe (2.5 ml). Stirred 22 h. at room temp., cooled to 0-3 deg.C., dild. with THF (5 ml), added 1 ml H2O, and stirred 15 min. Added kiesel-guhr (1 g), warmed to 20-5 deg.C., dried (2.5 g Na2SO4), and filtered, washing with 1:3 THF -PhMe (60 ml). Evapd. in vac., residue dissolved in PhH (16 ml), and hexane (144 ml), and chromatographed on Al2O3 activity IV (20 g), eluting with 9:1 and 8.5:1.5 hexane/PhH, to give I (153 mg) m.p. 212-6 deg.C (from Et2O-THF).</p> |