反応 #4094019
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-1ae6012641ae4eb2a1d77a829d2d70ab表示可能な構造データがありません
C1CN(CCN1)C2=C(C=CC=C2Cl)Cl製品情報
1-(2,6-dichlorophenyl)piperazine (CAS 63386-61-8) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 11492345
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
12 反応 · 12 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-1ae6012641ae4eb2a1d77a829d2d70ab反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of the benzoimidazole from step (c) above (75 mg, 0.34 mmol), the piperazine from step (a) above (90 mg, 0.39 mmol) and N,N-diisopropylethylamine (0.1 mL, 0.58 mmol, Aldrich) in DMSO (2 mL) was stirred at 80° C. for 24 h. The mixture was cooled to room temperature, water (10 mL) was added and the mixture was extracted with EtOAc (2×20 mL). The combined organic phases were washed with water (2×10 mL) and brine (5 mL), dried over Na2SO4, and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 20% EtOAc/hexane to give the title compound as a white solid. M.p. 263-265° C. MS (ESI, pos. ion) m/z: 415 (M+1). the mixture was extracted with EtOAc (2×20 mL) The combined organic phases were washed with water (2×10 mL) and brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 20% EtOAc/hexane
ソース ID: ord-d733d12a73de412484663657742d8122反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 2,6-dichlorophenylaniline (810 mg, 5 mmol, Aldrich) and bis(2-chloroethyl)amine hydrochloride (823 mg, 5 mmol, Aldrich) was subjected to microwave irradiation at 200° C. for 10 min. The reaction mixture was allowed to cool to room temperature then treated with 5N NaOH (5 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with brine (5 mL), dried over Na2SO4 and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water) to give the title compound. MS (ESI, pos. ion) m/z: 231 (M+1). irradiation at 200° C. for 10 min extracted with EtOAc (2×20 mL) The combined organic extracts were washed with brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water)
ソース ID: ord-7739c52eccd04b9bb90ee009de2421c2反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 2,6-dichlorophenylaniline (810 mg, 5 mmol, Aldrich) and bis(2-chloroethyl)amine hydrochloride (823 mg, 5 mmol, Aldrich) was subjected to microwave irradiation at 200° C. for 10 min. The reaction mixture was allowed to cool to room temperature then treated with 5N NaOH (5 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with brine (5 mL), dried over Na2SO4 and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water) to give the title compound. MS (ESI, pos. ion) m/z: 231 (M+1). irradiation at 200° C. for 10 min extracted with EtOAc (2×20 mL) The combined organic extracts were washed with brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water)
ソース ID: ord-7739c52eccd04b9bb90ee009de2421c2反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of the benzoimidazole from step (c) above (75 mg, 0.34 mmol), the piperazine from step (a) above (90 mg, 0.39 mmol) and N,N-diisopropylethylamine (0.1 mL, 0.58 mmol, Aldrich) in DMSO (2 mL) was stirred at 80° C. for 24 h. The mixture was cooled to room temperature, water (10 mL) was added and the mixture was extracted with EtOAc (2×20 mL). The combined organic phases were washed with water (2×10 mL) and brine (5 mL), dried over Na2SO4, and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 20% EtOAc/hexane to give the title compound as a white solid. M.p. 263-265° C. MS (ESI, pos. ion) m/z: 415 (M+1). the mixture was extracted with EtOAc (2×20 mL) The combined organic phases were washed with water (2×10 mL) and brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 20% EtOAc/hexane
ソース ID: ord-18db05cfa2954c4b856ff9818bcadebf反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 2,6-dichlorophenylaniline (810 mg, 5 mmol, Aldrich) and bis(2-chloroethyl)amine hydrochloride (823 mg, 5 mmol, Aldrich) was subjected to microwave irradiation at 200° C. for 10 min. The reaction mixture was allowed to cool to room temperature then treated with 5N NaOH (5 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with brine (5 mL), dried over Na2SO4 and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water) to give the title compound. MS (ESI, pos. ion) m/z: 231 (M+1). irradiation at 200° C. for 10 min extracted with EtOAc (2×20 mL) The combined organic extracts were washed with brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water)
ソース ID: ord-d0cb24a0527c42b2be03c7b3317efa64反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 2,6-dichlorophenylaniline (810 mg, 5 mmol, Aldrich) and bis(2-chloroethyl)amine hydrochloride (823 mg, 5 mmol, Aldrich) was subjected to microwave irradiation at 200° C. for 10 min. The reaction mixture was allowed to cool to room temperature then treated with 5N NaOH (5 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with brine (5 mL), dried over Na2SO4 and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water) to give the title compound. MS (ESI, pos. ion) m/z: 231 (M+1). irradiation at 200° C. for 10 min extracted with EtOAc (2×20 mL) The combined organic extracts were washed with brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water)
ソース ID: ord-d0cb24a0527c42b2be03c7b3317efa64反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-1ae6012641ae4eb2a1d77a829d2d70ab反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Phenyl-N-(5-ethyl-2-methoxy-6-methylpyridin-3-yl)carbamate and 1-(2,6-dichlorophenyl)piperazine were reacted by the same way with the example 1 to obtain the titled compound.
ソース ID: ord-93b00721b64648168c8aa7cf99a62ca6反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of the benzoimidazole from step (c) above (75 mg, 0.34 mmol), the piperazine from step (a) above (90 mg, 0.39 mmol) and N,N-diisopropylethylamine (0.1 mL, 0.58 mmol, Aldrich) in DMSO (2 mL) was stirred at 80° C. for 24 h. The mixture was cooled to room temperature, water (10 mL) was added and the mixture was extracted with EtOAc (2×20 mL). The combined organic phases were washed with water (2×10 mL) and brine (5 mL), dried over Na2SO4, and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 20% EtOAc/hexane to give the title compound as a white solid. M.p. 263-265° C. MS (ESI, pos. ion) m/z: 415 (M+1). the mixture was extracted with EtOAc (2×20 mL) The combined organic phases were washed with water (2×10 mL) and brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 20% EtOAc/hexane
ソース ID: ord-d733d12a73de412484663657742d8122反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 2,6-dichlorophenylaniline (810 mg, 5 mmol, Aldrich) and bis(2-chloroethyl)amine hydrochloride (823 mg, 5 mmol, Aldrich) was subjected to microwave irradiation at 200° C. for 10 min. The reaction mixture was allowed to cool to room temperature then treated with 5N NaOH (5 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with brine (5 mL), dried over Na2SO4 and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water) to give the title compound. MS (ESI, pos. ion) m/z: 231 (M+1). irradiation at 200° C. for 10 min extracted with EtOAc (2×20 mL) The combined organic extracts were washed with brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 10% MeOH/CH2Cl2+1% ammonia (30% in water)
ソース ID: ord-7739c52eccd04b9bb90ee009de2421c2反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of the benzoimidazole from step (c) above (75 mg, 0.34 mmol), the piperazine from step (a) above (90 mg, 0.39 mmol) and N,N-diisopropylethylamine (0.1 mL, 0.58 mmol, Aldrich) in DMSO (2 mL) was stirred at 80° C. for 24 h. The mixture was cooled to room temperature, water (10 mL) was added and the mixture was extracted with EtOAc (2×20 mL). The combined organic phases were washed with water (2×10 mL) and brine (5 mL), dried over Na2SO4, and filtered. The solvent was removed in vacuo and the residue was purified by silica gel chromatography, eluting with 20% EtOAc/hexane to give the title compound as a white solid. M.p. 263-265° C. MS (ESI, pos. ion) m/z: 415 (M+1). the mixture was extracted with EtOAc (2×20 mL) The combined organic phases were washed with water (2×10 mL) and brine (5 mL) dried over Na2SO4 filtered The solvent was removed in vacuo the residue was purified by silica gel chromatography eluting with 20% EtOAc/hexane
ソース ID: ord-18db05cfa2954c4b856ff9818bcadebfPubChem References
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