(±)-3-溴-1-苯基-2-吡咯烷

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

实验步骤: A solution of 60.1 mg (0.23 mmol) of the compound from example 1g in 1 ml of absolute DMF was mixed with 11 mg (0.23 mmol) of sodium hydride (50%) and stirred at RT for 1 h. Then 55.5 mg (0.23 mmol) of (+/−)-3-bromo-1-phenyl-2-pyrrolidinone were added, and the mixture was stirred at RT for 45 min. The reaction solution was mixed with 1 ml of water and extracted several times with EA. The combined EA extracts were dried over Na2SO4, filtered and concentrated. Purification of the resulting residue by chromatography on silica gel with CH2Cl2/methanol (92:8 to 85:15 in 35 min) as mobile phase afforded 52.2 mg of the title compound. the mixture was stirred at RT for 45 min extracted several times with EA The combined EA extracts were dried over Na2SO4 filtered concentrated Purification of the resulting residue by chromatography on silica gel with CH2Cl2/methanol (92:8 to 85:15 in 35 min) as mobile phase

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

实验步骤: To a suspension of phenylamine L (465 mg, 5.0 mmol) and potassium phosphate (530 mg, 2.5 mmol) in acetonitrile (20 mL) was added 2,4-dibromo-butyryl chloride III (1.32 g, 5.0 mmol) at 0° C. The mixture was brought to rt and stirred for 1 hr. Then NaOH (1 mL, 50% aqueous solution) was added, and the mixture was stirred overnight. After the mixture was filtered, the solid was washed with acetonitrile (10 mL), and the combined filtrate was concentrated. The residue was purified by column chromatography (eluate: EtOAc/petroleum ether from 1/5 to 1/3) to afford 3-bromo-1-phenyl-pyrrolidin-2-one LI as white solid. was brought to rt the mixture was stirred overnight After the mixture was filtered the solid was washed with acetonitrile (10 mL) the combined filtrate was concentrated The residue was purified by column chromatography (eluate: EtOAc/petroleum ether from 1/5 to 1/3)