1-(2-甲氧基苯基)-1,4-二氮杂

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 1-(2-Methoxy-phenyl)-[1,4]diazepane (103 mg, 0.5 mmol), 4-(5-fluoro-1H-3-indolyl)-cyclohexanone (116 mg, 0.5 mmol) 5 mL 1,2-dichloroethane and 159 mg (0.75 mmol) of NaBH(OAc), were stirred at 23° C. in a 20 mL scintillation vial for 21 h. The reaction was quenched with 2 mL 1N NaOH, the vial capped, shaken and the organic layer (bottom layer) was removed with an automatic pipet. The organics were removed in a Speed Vac and pumped down overnight to afford 169 mg (0.4 mmol, an 80% yield) of the title compound as an off-white solid. MS (ES) m/z (relative intensity): 422 (M++H, 100). The reaction was quenched with 2 mL 1N NaOH the organic layer (bottom layer) was removed with an automatic pipet The organics were removed in a Speed Vac to afford 169 mg (0.4 mmol

反应条件: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 2.03 g (6.62 mmol) of 4-(2-methoxy-phenyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester in 30 mL CH2Cl2 at 23° C. was added 5 mL trifluoroacetic acid. After stirring at 23° C. for 30 min, 4 additional mL of trifluoroacetic acid were added. After a total of 1 h, the reaction solution was poured into 200 mL of saturated aqueous NaHCO3 and extracted with 3×100 mL of EtOAc. The combined organics were washed with 1×200 mL H2O, 1×200 mL brine, dried over Na2SO4, filtered and evaporated to give 1.01 g (4.90 mmol, a 74% yield) of the title compound as a yellow oil. 1H NMR (300 MHz, CDCl3): δ1.99 (pent, J=4.5 Hz, 2H), 2.82 (brs, 1H), 3.06 (t, J=4.4 Hz, 2H), 3.08-3.13 (m, 2H), 3.29-3.36 (m, 4H), 3.84 (s, 3H), 6.83-6.96 (m, 4H); IR (KBr, cm−1): 3335w;, MS (ES) m/z (relative intensity): 207 (M++H, 100). extracted with 3×100 mL of EtOAc The combined organics were washed with 1×200 mL H2O, 1×200 mL brine dried over Na2SO4 filtered evaporated to give 1.01 g (4.90 mmol