反応 #4017906
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-2ff86549af0940e7b8e78b6034bb8a49表示可能な構造データがありません
C1CN(CCC1CCl)CC2=CC=CC=C2製品情報
1-benzyl-4-(chloromethyl)piperidine (CAS 136704-10-4) 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 430959
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
6 反応 · 6 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2ff86549af0940e7b8e78b6034bb8a49反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Sodium hydride (1.69 g, 42.1 mmol; 80% dispersion in oil) was added portionwise over 10 minutes to a solution of diphenylacetonitrile (7.4 g, 38.3 mmol) in toluene (40 ml) and the mixture was heated under reflux for 45 minutes, treated with 1-benzyl-4-chloromethylpiperidine (4.3 g, 1.92 mmol; prepared by partitioning the hydrochloride salt, which was obtained by the method described in J. Het. Chem., 1978, 15, 675, between 10% aqueous sodium carbonate solution and dichloromethane, drying the organic layer over magnesium sulphate and evaporating), heated under reflux for one hour, allowed to cool to room temperature and partitioned between toluene and water. The organic layer was dried over magnesium sulphate and evaporated. The residue was purified by chromatography on silica using dichloromethane plus 0-5% methanol as eluant. Appropriate fractions were combined and evaporated to give the title compound (7.57 g, 52%) as a colourless foam which was characterised by its 1H-NMR spectrum. the mixture was heated under reflux for 45 minutes prepared by partitioning the hydrochloride salt which was obtained by the method , 1978, 15, 675, between 10% aqueous sodium carbonate solution and dichloromethane, drying the organic layer over magnesium sulphate evaporating), heated under reflux for one hour partitioned between toluene and water The organic layer was dried over magnesium sulphate evaporated The residue was purified by chromatography on silica evaporated
ソース ID: ord-5c9f7cf20f8f447d8dfaf5dbab062990反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Sodium hydride (1.69 g, 42.1 mmol; 80% dispersion in oil) was added portionwise over 10 minutes to a solution of diphenylacetonitrile (7.4 g, 38.3 mmol) in toluene (40 ml) and the mixture was heated under reflux for 45 minutes, treated with 1-benzyl-4-chloromethylpiperidine (4.3 g, 1.92 mmol; prepared by partitioning the hydrochloride salt, which was obtained by the method described in J. Het. Chem., 1978, 15, 675, between 10% aqueous sodium carbonate solution and dichloromethane, drying the organic layer over magnesium sulphate and evaporating), heated under reflux for one hour, allowed to cool to room temperature and partitioned between toluene and water. The organic layer was dried over magnesium sulphate and evaporated. The residue was purified by chromatography on silica using dichloromethane plus 0-5% methanol as eluant. Appropriate fractions were combined and evaporated to give the title compound (7.57 g, 52%) as a colourless foam which was characterised by its 1H-NMR spectrum. the mixture was heated under reflux for 45 minutes prepared by partitioning the hydrochloride salt which was obtained by the method , 1978, 15, 675, between 10% aqueous sodium carbonate solution and dichloromethane, drying the organic layer over magnesium sulphate evaporating), heated under reflux for one hour partitioned between toluene and water The organic layer was dried over magnesium sulphate evaporated The residue was purified by chromatography on silica evaporated
ソース ID: ord-5c9f7cf20f8f447d8dfaf5dbab062990反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2ff86549af0940e7b8e78b6034bb8a49反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Sodium hydride (1.69 g, 42.1 mmol; 80% dispersion in oil) was added portionwise over 10 minutes to a solution of diphenylacetonitrile (7.4 g, 38.3 mmol) in toluene (40 ml) and the mixture was heated under reflux for 45 minutes, treated with 1-benzyl-4-chloromethylpiperidine (4.3 g, 1.92 mmol; prepared by partitioning the hydrochloride salt, which was obtained by the method described in J. Het. Chem., 1978, 15, 675, between 10% aqueous sodium carbonate solution and dichloromethane, drying the organic layer over magnesium sulphate and evaporating), heated under reflux for one hour, allowed to cool to room temperature and partitioned between toluene and water. The organic layer was dried over magnesium sulphate and evaporated. The residue was purified by chromatography on silica using dichloromethane plus 0-5% methanol as eluant. Appropriate fractions were combined and evaporated to give the title compound (7.57 g, 52%) as a colourless foam which was characterised by its 1H-NMR spectrum. the mixture was heated under reflux for 45 minutes prepared by partitioning the hydrochloride salt which was obtained by the method , 1978, 15, 675, between 10% aqueous sodium carbonate solution and dichloromethane, drying the organic layer over magnesium sulphate evaporating), heated under reflux for one hour partitioned between toluene and water The organic layer was dried over magnesium sulphate evaporated The residue was purified by chromatography on silica evaporated
ソース ID: ord-5c9f7cf20f8f447d8dfaf5dbab062990反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2ff86549af0940e7b8e78b6034bb8a49PubChem References
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