| 摘要 |
<p>Method for Aldosterone inhibitor. (a) BF3-Et2O (13.3 ml.) was added (30 min) to NaBH4 (2.99g) in THF (63 ml.) and 2-methylbut-2-ene (22.3 ml.) at -5 to -10 deg. under N2, stirred 30 min. at 0 deg., and 2 1/2 h. at 25 deg., giving a soln. of di-i-amyl borane. II (9.9 g.) in THF (42 ml.) was added to this at -15 to -20 deg., stirred 4 h. at 0 deg., cooled to -15 deg., and added 3N-NaOH (32 ml) fast enough to raise the temp. to 0 deg., and then 30% H2O2 (32 ml.), raising the temp. to 25 - 30 deg. Stirred 1 1/2 h. at 20 deg., dild. with 15% NaHSO3 soln., the THF removed in vac., filtered and washed. The residue was refluxed in CHCl3 (200 ml.), giving III (10.2g.), m.p. 275 - 8 deg.</p> |
