| 摘要 |
Method for R = lower alkyl R' = H, hal, NO2 or CF3 R2 = H or hal Intermediates for 2,3,4,5-tetrahydro-1,4-benzodiazepines (II) with anti-convulsant, muscle relaxant, and sedative activity. 98% HCO2H (100 ml) was added to N-(p-chlorophenyl)-N-methyl-ethylenediamine (70 g.) at 0 deg., followed by PhCHO (40 g.) at 25 deg. The mixture was heated 17 h. at 95 deg., cooled, poured into an ice-Et2O-3N NaOH mixture, sepd., and the H2O phase extd. with Et2O (3X100 ml). The Et2O was washed with H2O, dried, evapd., the oily residue dissolved in N-HCl (500 ml) and Et2O (250 ml), the Et2O sepd., the H2O phase extd. with Et2O (3X250 ml) and the combined Et2O dried, evapd., and recryst. from PriOH, giving I, m.p.120-121 deg. |
