反应详情

Treat 1-(4-Chlorophenyl)-2-isopropyl-2,7-diazaspiro[3.5]nonane, Isomer A (0.015 g) in ClCH2CH2Cl (1 mL) and acetonitrile (1 mL) with cycloheptyl isocyanate (18 uL), and the resulting mixture stirred at RT for 424 h. P—S Trisamine (Argoonaut, 4.64 mmol/g) (120 g) and ClCH2CH2Cl (2 mL) were added and the resulting mixture was shaken to 20 h. The reaction mixture was filtered, the resin washed with CH2Cl2 (2 mL). The resulting filtrate was concentrated in vacuo and then placed on a silica gel plate (1000 u) and eluted with CH2Cl2:MeOH (95:5) to give of 1-(4-chlorophenyl)-2-isopropyl-2,7-diazaspiro[3.5]nonane-7-carboxamide, white residue (0.0208 g). Add MeOH (0.5 mL) and 0.1N HCl in MeOH (1 mL), and concentrate in vacuo to give the title compound, as a white solid (0.0222 g).

1. filtrationThe reaction mixture was filtered
2. washthe resin washed with CH2Cl2 (2 mL)
3. concentrationThe resulting filtrate was concentrated in vacuo
4. washeluted with CH2Cl2:MeOH (95:5)