| 摘要 |
<p>Cpds. I and II, their 5alpha-H and 6-dehydro analogues, acid addn. salts, and pharm. prepns. contg. them. where R1 = H, beta-OH, beta-Cl, or O, but may only be H or halogen if X is H or halogen respectively R2 = H, alpha-Me, or alpha-F R3 = H, alpha-Me, beta-Me, or R4 = H, alkyl, aralkyl, cycloalkyl, aryl, acyl, or an opt. substd. heterocyclic residue X = H or halogen. Anti-inflammatories. IV (R1 = 11beta-OH, R2 = R3 = X = Hf 1.35 g) in PhH (23 ml), was treated at 25 deg.C with HCO2Et (0.96 ml). Purged with N2, added NaH (560 mg) as 58% dispersion in oil, stirred overnight, and poured into sat. NaH2PO4 soln. Extd. with PhH(4 X), washed with H2O (3 X), dried, evapd., and purified via the Na salt, giving V. To V (850 mg) in EtOH (9.2 ml) was added N2H4.H2O (0.16 ml) in EtOH (0.16 ml). Refluxed 45 min. under N2, evapd. in vac., washed (3 X H2O) and dried in vac. at 80 deg.C., giving VI (R4 = H). This cpd. (720 mg) heated 30 min. at 100 deg. in 60% HCHO (24 ml), evapd. in vac., at 50 deg.C., dried at 60 deg. in vac., giving II + the formyl deriv. This mixture (0.5 g) in MeOH (2.4 ml) was treated with 1.33N - NaOMe (0.9 ml) for 10 min. at 25 deg.C under N2. Neutralised, evapd. in vac., washed with hexane and with H2O, and dried, giving II.</p> |
