2-氨基苯丙酮

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

实验步骤: A 2.0N solution of ethylmagnesium chloride in THF (100 ml) was cooled to 0° C. under nitrogen atmosphere, and thereto was added dropwise a solution of 2-cyanoaniline (7.90 g) in THF (65 ml) over a period of 50 minutes. The mixture was stirred at room temperature for 20 minutes, and refluxed for 3 hours. The reaction solution was cooled to 0° C., and thereto was added a 4N aqueous hydrochloric acid solution (80 ml) over a period of 40 minutes, and the mixture was further refluxed for 3 hours. The solvent in the reaction solution was evaporated under reduced pressure, and the resultant was added to a saturated aqueous sodium hydrogen carbonate solution for neutralization. The mixture was extracted three times with ethyl acetate, and the extract was washed with a saturated brine, dried over magnesium sulfate, and filtered. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column (hexane/ethyl acetate=8/1) to give 1-(2-aminophenyl)-1-propanone (6.78 g, 68%). refluxed for 3 hours The reaction solution was cooled to 0° C. the mixture was further refluxed for 3 hours The solvent in the reaction solution was evaporated under reduced pressure the resultant was added to a saturated aqueous sodium hydrogen carbonate solution for neutralization The mixture was extracted three times with ethyl acetate the extract was washed with a saturated brine dried over magnesium sulfate filtered The solvent was evaporated under reduced pressure the residue was purified by silica gel column (hexane/ethyl acetate=8/1)

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

实验步骤: To a mixture of 1-(2-aminophenyl)propan-1-one (CAS1196-28-7) (4.6 g), monobenzyl malonate (7.2 g), and THF (46 mL) were added EDC.HCl (7.1 g) and HOBt.H2O (7.1 g), and the mixture was stirred at room temperature for 14 h and then heated to reflux for 8 h. The solvent was evaporated under reduced pressure, and the residue was diluted with ethyl acetate and then washed with saturated aqueous sodium hydrogencarbonate and saturated brine. The organic layer was dried with anhydrous sodium sulfate, the desiccant was removed by filtration, then the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=9:1) to obtain benzyl N-(2-propionylphenyl)malonamate (1.8 g). heated to reflux for 8 h The solvent was evaporated under reduced pressure the residue was diluted with ethyl acetate washed with saturated aqueous sodium hydrogencarbonate and saturated brine The organic layer was dried with anhydrous sodium sulfate the desiccant was removed by filtration the filtrate was concentrated under reduced pressure the residue was purified by silica gel column chromatography (hexane/ethyl acetate=9:1)

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

实验步骤: 2-Aminobenzonitrile (1 mmol) was disposed in anhydrous tetrahydrofuran (5 ml) is followed by adding ethylmagnesium bromide (10 equivalent weights) at 0° C. under nitrogen gas atmosphere and reacting for 4 hours to obtain a reaction product. The pH of the reaction product was adjusted to be in the range of 3 to 4 using 1N HCl, followed by partitioning using ethyl acetate and saturated NaHCO3 for three times. The ethyl acetate layer was collected and purified using a silica gel column (n-hexane/acetone=4:1), thereby obtaining [1-(2-aminophenyl)propan-1-one] (83.5 mg, yield 56%). to obtain a reaction product by partitioning The ethyl acetate layer was collected purified