反応 #4074756
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-c48a18fc64194fd4afedbd6f39164b4e表示可能な構造データがありません
CC(OC(N1CCC(CN2CCNCC2)CC1)=O)(C)C製品情報
381722-48-1 (CAS 381722-48-1) 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 22321697
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
9 反応 · 9 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-c48a18fc64194fd4afedbd6f39164b4e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirring solution of 1-Boc-piperidine-4-carboxaldehyde (2.4 g, 11.3 mmol) in THF (60 mL) and acetonitrile (15 mL) was added piperazine (4.85 g, 56.3 mmol). After stirring for 5 h, sodium triacetoxyborohydride (2.87 g, 13.5 mmol) was added and the reaction was allowed to stir overnight. The next morning, the solvents were removed by rotary evaporation and the residue was dissolved in ethyl acetate, washed twice with satd aq. NaHCO3, followed by water, then dried over MgSO4, filtered and concentrated in vacuo. The residue was then chromatographed over silica gel, eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane. The product containing fractions were combined and concentrated in vacuo to give 4.03 g (48%) of the title compound. to stir overnight The next morning, the solvents were removed by rotary evaporation the residue was dissolved in ethyl acetate washed twice with satd aq. NaHCO3 dried over MgSO4 filtered concentrated in vacuo The residue was then chromatographed over silica gel eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane The product containing fractions concentrated in vacuo
ソース ID: ord-fe044173d09d4a38a2bc976ea0c9e215反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirring solution of 1-Boc-piperidine-4-carboxaldehyde (2.4 g, 11.3 mmol) in THF (60 mL) and acetonitrile (15 mL) was added piperazine (4.85 g, 56.3 mmol). After stirring for 5 h, sodium triacetoxyborohydride (2.87 g, 13.5 mmol) was added and the reaction was allowed to stir overnight. The next morning, the solvents were removed by rotary evaporation and the residue was dissolved in ethyl acetate, washed twice with satd aq. NaHCO3, followed by water, then dried over MgSO4, filtered and concentrated in vacuo. The residue was then chromatographed over silica gel, eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane. The product containing fractions were combined and concentrated in vacuo to give 4.03 g (48%) of the title compound. to stir overnight The next morning, the solvents were removed by rotary evaporation the residue was dissolved in ethyl acetate washed twice with satd aq. NaHCO3 dried over MgSO4 filtered concentrated in vacuo The residue was then chromatographed over silica gel eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane The product containing fractions concentrated in vacuo
ソース ID: ord-7ead58d193574058a0a4b93e023c72b1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirring solution of 1-Boc-piperidine-4-carboxaldehyde (2.4 g, 11.3 mmol) in THF (60 mL) and acetonitrile (15 mL) was added piperazine (4.85 g, 56.3 mmol). After stirring for 5 h, sodium triacetoxyborohydride (2.87 g, 13.5 mmol) was added and the reaction was allowed to stir overnight. The next morning, the solvents were removed by rotary evaporation and the residue was dissolved in ethyl acetate, washed twice with satd aq. NaHCO3, followed by water, then dried over MgSO4, filtered and concentrated in vacuo. The residue was then chromatographed over silica gel, eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane. The product containing fractions were combined and concentrated in vacuo to give 4.03 g (48%) of the title compound. to stir overnight The next morning, the solvents were removed by rotary evaporation the residue was dissolved in ethyl acetate washed twice with satd aq. NaHCO3 dried over MgSO4 filtered concentrated in vacuo The residue was then chromatographed over silica gel eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane The product containing fractions concentrated in vacuo
ソース ID: ord-6a6a7affc65a43ef9d31035675e8db96反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirring solution of 1-Boc-piperidine-4-carboxaldehyde (2.4 g, 11.3 mmol) in THF (60 mL) and acetonitrile (15 mL) was added piperazine (4.85 g, 56.3 mmol). After stirring for 5 h, sodium triacetoxyborohydride (2.87 g, 13.5 mmol) was added and the reaction was allowed to stir overnight. The next morning, the solvents were removed by rotary evaporation and the residue was dissolved in ethyl acetate, washed twice with satd aq. NaHCO3, followed by water, then dried over MgSO4, filtered and concentrated in vacuo. The residue was then chromatographed over silica gel, eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane. The product containing fractions were combined and concentrated in vacuo to give 4.03 g (48%) of the title compound. to stir overnight The next morning, the solvents were removed by rotary evaporation the residue was dissolved in ethyl acetate washed twice with satd aq. NaHCO3 dried over MgSO4 filtered concentrated in vacuo The residue was then chromatographed over silica gel eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane The product containing fractions concentrated in vacuo
ソース ID: ord-6a6a7affc65a43ef9d31035675e8db96反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-c48a18fc64194fd4afedbd6f39164b4e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirring solution of 1-Boc-piperidine-4-carboxaldehyde (2.4 g, 11.3 mmol) in THF (60 mL) and acetonitrile (15 mL) was added piperazine (4.85 g, 56.3 mmol). After stirring for 5 h, sodium triacetoxyborohydride (2.87 g, 13.5 mmol) was added and the reaction was allowed to stir overnight. The next morning, the solvents were removed by rotary evaporation and the residue was dissolved in ethyl acetate, washed twice with satd aq. NaHCO3, followed by water, then dried over MgSO4, filtered and concentrated in vacuo. The residue was then chromatographed over silica gel, eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane. The product containing fractions were combined and concentrated in vacuo to give 4.03 g (48%) of the title compound. to stir overnight The next morning, the solvents were removed by rotary evaporation the residue was dissolved in ethyl acetate washed twice with satd aq. NaHCO3 dried over MgSO4 filtered concentrated in vacuo The residue was then chromatographed over silica gel eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane The product containing fractions concentrated in vacuo
ソース ID: ord-fe044173d09d4a38a2bc976ea0c9e215反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirring solution of 1-Boc-piperidine-4-carboxaldehyde (2.4 g, 11.3 mmol) in THF (60 mL) and acetonitrile (15 mL) was added piperazine (4.85 g, 56.3 mmol). After stirring for 5 h, sodium triacetoxyborohydride (2.87 g, 13.5 mmol) was added and the reaction was allowed to stir overnight. The next morning, the solvents were removed by rotary evaporation and the residue was dissolved in ethyl acetate, washed twice with satd aq. NaHCO3, followed by water, then dried over MgSO4, filtered and concentrated in vacuo. The residue was then chromatographed over silica gel, eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane. The product containing fractions were combined and concentrated in vacuo to give 4.03 g (48%) of the title compound. to stir overnight The next morning, the solvents were removed by rotary evaporation the residue was dissolved in ethyl acetate washed twice with satd aq. NaHCO3 dried over MgSO4 filtered concentrated in vacuo The residue was then chromatographed over silica gel eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane The product containing fractions concentrated in vacuo
ソース ID: ord-7ead58d193574058a0a4b93e023c72b1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a stirring solution of 1-Boc-piperidine-4-carboxaldehyde (2.4 g, 11.3 mmol) in THF (60 mL) and acetonitrile (15 mL) was added piperazine (4.85 g, 56.3 mmol). After stirring for 5 h, sodium triacetoxyborohydride (2.87 g, 13.5 mmol) was added and the reaction was allowed to stir overnight. The next morning, the solvents were removed by rotary evaporation and the residue was dissolved in ethyl acetate, washed twice with satd aq. NaHCO3, followed by water, then dried over MgSO4, filtered and concentrated in vacuo. The residue was then chromatographed over silica gel, eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane. The product containing fractions were combined and concentrated in vacuo to give 4.03 g (48%) of the title compound. to stir overnight The next morning, the solvents were removed by rotary evaporation the residue was dissolved in ethyl acetate washed twice with satd aq. NaHCO3 dried over MgSO4 filtered concentrated in vacuo The residue was then chromatographed over silica gel eluting with a step gradient of 2% through 15% (2 N ammonia/methanol) in dichloromethane The product containing fractions concentrated in vacuo
ソース ID: ord-6a6a7affc65a43ef9d31035675e8db96PubChem References
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