1-(3-chloropropyl)pyrrolidin-2-one

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-chloro-3-[2-oxopyrrolidin-1-yl]propane (2.0 g, 12.0 mmol), 1-(4-ethylphenyl)piperazine (2.36 g, 12.0 mmol), anhydrous Na2CO3 (0.658 g, 6.2 mmol) and NaI (0.18 g, 1.2 mmol) in dry DMF (10 ml) was stirred at 80° C. for 12 hrs. The reaction mixture was cooled, poured on water (30 ml) and the separated residue was extracted with CHCl3 (2×30 ml). The extracts were dried over Na2So4 and concentrated under reduced pressure to give 1-[4-(4-ethylphenyl)piperazin-1-yl]-3-[2-oxopyrrolidin-1-yl]propane as an oil which was purified by flash column chromatography over silica gel using chloroform as eluent, yield 2.43 g (62.0%). IR (Neat): 2940, 2800, 1660, 1440, 1000, 900,800. 1H NMR (CDCl3): 1.20(t, 3H, J=6.0 Hz, CH2CH3, 1.60-280(m, 14H, 3',4',2,1 & 2×N--CH2, CH2CH3), 3.00-3.60(m, 8H, 5', 3 & 2×N--CH2). MS: m/z 315 (M+). The reaction mixture was cooled poured on water (30 ml) the separated residue was extracted with CHCl3 (2×30 ml) The extracts were dried over Na2So4 concentrated under reduced pressure

反応条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-chloro-3-[2-oxopyrrolidin-1-yl]propane (1 g, 6.2 mmcl), 1-(3-chlorophenyl)piperazine (1.22 g, 6.2 minol) anhydrous Na2CO3 (0.33 g, 3.1 mmol) and Nal (0.093 g, 0.6 mmcl) in dry xylene (15 ml) was stirred at 150° C. for 14 hours. The solvent was removed at reduced pressure and residue was poured on water (30 ml). The separated residue was extracted with dichloromethane (2×25 ml), dried over Na2SO4 and concentrated to give 1-[4-(3-chlorophenyl)piperazin-1-yl]-3-[3-oxopyrrolidin-1-yl]propane as an oil which was purified by flash column chromatography over silica gel using chloroform as fluent, yield 0.72 g (36%). The solvent was removed at reduced pressure and residue was poured on water (30 ml) The separated residue was extracted with dichloromethane (2×25 ml) dried over Na2SO4 concentrated

反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-chloro-3-[2-oxopyrrolidin-1-yl]propane (1.0 g, 6.2 mmol), 1-(3-chlorophenyl)piperazine (1.22 g, 6.2 minol), anhydrous Na2CO3 (0.33 g, 3.1 mmol) and Nal (0.093 g, 0.6 mmcl) in dry toluene (10 ml) was stirred at 110° C. for 12 hrs. The solvent was removed at reduced pressure and residue was poured on water (20 ml). The separated residue was extracted with ethylacetate (3×20 ml), dried over Na2SO4 and concentrated under reduced pressure to give 1-[4-(3-chlorophenyl)piperazin-1-yl]-3-[2-oxopyrrolidin-1-yl]propane as an oil which was purified by flash column chromatography over silica gel using chloroform as eluent, yield 0.60 g (30.0%). The solvent was removed at reduced pressure and residue was poured on water (20 ml) The separated residue was extracted with ethylacetate (3×20 ml) dried over Na2SO4 concentrated under reduced pressure

反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-chloro-3-[2-oxopyrrolidin-1-yl]propane (1.0 g, 6.2 mmol), 1-(3-chlorophenyl)piperazine (1.22 g, 6.2 minol), anhydrous Na2CO3 (0.33 g, 3.1 mmol) and Nal (0.093 g, 0.6 mmcl) in dry toluene (10 ml) was stirred at 110° C. for 12 hrs. The solvent was removed at reduced pressure and residue was poured on water (20 ml). The separated residue was extracted with ethylacetate (3×20 ml), dried over Na2SO4 and concentrated under reduced pressure to give 1-[4-(3-chlorophenyl)piperazin-1-yl]-3-[2-oxopyrrolidin-1-yl]propane as an oil which was purified by flash column chromatography over silica gel using chloroform as eluent, yield 0.60 g (30.0%). The solvent was removed at reduced pressure and residue was poured on water (20 ml) The separated residue was extracted with ethylacetate (3×20 ml) dried over Na2SO4 concentrated under reduced pressure

反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 1-chloro-3-[2-oxopyrrolidin-1-yl]propane (1.0 g, 6.2 mmol), 1-(3-chlorophenyl)piperazine (1.22 g, 6.2 minol), anhydrous Na2CO3 (0.33 g, 3.1 mmol) and Nal (0.093 g, 0.6 mmcl) in dry toluene (10 ml) was stirred at 110° C. for 12 hrs. The solvent was removed at reduced pressure and residue was poured on water (20 ml). The separated residue was extracted with ethylacetate (3×20 ml), dried over Na2SO4 and concentrated under reduced pressure to give 1-[4-(3-chlorophenyl)piperazin-1-yl]-3-[2-oxopyrrolidin-1-yl]propane as an oil which was purified by flash column chromatography over silica gel using chloroform as eluent, yield 0.60 g (30.0%). The solvent was removed at reduced pressure and residue was poured on water (20 ml) The separated residue was extracted with ethylacetate (3×20 ml) dried over Na2SO4 concentrated under reduced pressure