反应 #3847010
相关文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-ae128cf97265439c98bd5515384f376b暂无可渲染的结构数据
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7 条反应 · 7 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-ae128cf97265439c98bd5515384f376b反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: LAH (1.04 g, 0.0273 mol, 3.0 eq) was dissolved in THF (25 ml), and to this solution was added dropwise a THF solution (25 ml) of (2-benzyloxyphenyl)-acetonitrile (2.04 g, 0.0091 mol, 1.0 eq) under ice-cooling. After the completion of the dropwise addition, the mixture was stirred at room temperature for 15 minutes and refluxed under heating for 2 hours. This reaction mixture was cooled with ice-cold water, and a saturated aqueous sodium sulfate solution (about 30-40 ml) was added. After filtration through Celite, the filtrate was concentrated under reduced pressure. The obtained residue was purified by column chromatography (chloroforn/methanol=5/1) to give 2-(2-benzyloxyphenyl)ethylamine (0.415 g, 20.0%) as a pale-yellow amorphous compound. cooling After the completion of the dropwise addition refluxed under heating for 2 hours This reaction mixture was cooled with ice-cold water After filtration through Celite the filtrate was concentrated under reduced pressure The obtained residue was purified by column chromatography (chloroforn/methanol=5/1)
来源 ID: ord-c56bc94ff2694cb0891615538ed13200反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: (2-Hydro xyphenyl)acetonitrile (1.01 g, 0.0076 mol) was dissolved in DMF (10 ml), and to this solution were successively added benzyl bromide (0.90 ml, 0.0076 mol, 1.0 eq) and anhydrous potassium carbonate (2.1 g, 0.015 mol, 3.0 eq). The mixture was stirred with heating at 90° C. for 1.5 hours. The reaction mixture was cooled to room temperature, and water (10 ml) was added. The mixture was extracted twice with ethyl acetate (30 ml). The organic layers were combined, washed with saturated brine (60 ml) and dried over anhydrous sodium sulfate. The drying agent was filtered off, and the filtrate was concentrated under reduced pressure to give (2-benzyloxyphenyl)acetonitrile (2.04 g, 100%) as a colorless solid. The reaction mixture was cooled to room temperature The mixture was extracted twice with ethyl acetate (30 ml) washed with saturated brine (60 ml) dried over anhydrous sodium sulfate The drying agent was filtered off the filtrate was concentrated under reduced pressure
来源 ID: ord-65b7b6d8a6394ec7a3867682c8823ee2反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: (2-Hydro xyphenyl)acetonitrile (1.01 g, 0.0076 mol) was dissolved in DMF (10 ml), and to this solution were successively added benzyl bromide (0.90 ml, 0.0076 mol, 1.0 eq) and anhydrous potassium carbonate (2.1 g, 0.015 mol, 3.0 eq). The mixture was stirred with heating at 90° C. for 1.5 hours. The reaction mixture was cooled to room temperature, and water (10 ml) was added. The mixture was extracted twice with ethyl acetate (30 ml). The organic layers were combined, washed with saturated brine (60 ml) and dried over anhydrous sodium sulfate. The drying agent was filtered off, and the filtrate was concentrated under reduced pressure to give (2-benzyloxyphenyl)acetonitrile (2.04 g, 100%) as a colorless solid. The reaction mixture was cooled to room temperature The mixture was extracted twice with ethyl acetate (30 ml) washed with saturated brine (60 ml) dried over anhydrous sodium sulfate The drying agent was filtered off the filtrate was concentrated under reduced pressure
来源 ID: ord-65b7b6d8a6394ec7a3867682c8823ee2反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-ae128cf97265439c98bd5515384f376b反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: LAH (1.04 g, 0.0273 mol, 3.0 eq) was dissolved in THF (25 ml), and to this solution was added dropwise a THF solution (25 ml) of (2-benzyloxyphenyl)-acetonitrile (2.04 g, 0.0091 mol, 1.0 eq) under ice-cooling. After the completion of the dropwise addition, the mixture was stirred at room temperature for 15 minutes and refluxed under heating for 2 hours. This reaction mixture was cooled with ice-cold water, and a saturated aqueous sodium sulfate solution (about 30-40 ml) was added. After filtration through Celite, the filtrate was concentrated under reduced pressure. The obtained residue was purified by column chromatography (chloroforn/methanol=5/1) to give 2-(2-benzyloxyphenyl)ethylamine (0.415 g, 20.0%) as a pale-yellow amorphous compound. cooling After the completion of the dropwise addition refluxed under heating for 2 hours This reaction mixture was cooled with ice-cold water After filtration through Celite the filtrate was concentrated under reduced pressure The obtained residue was purified by column chromatography (chloroforn/methanol=5/1)
来源 ID: ord-c56bc94ff2694cb0891615538ed13200反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: (2-Hydro xyphenyl)acetonitrile (1.01 g, 0.0076 mol) was dissolved in DMF (10 ml), and to this solution were successively added benzyl bromide (0.90 ml, 0.0076 mol, 1.0 eq) and anhydrous potassium carbonate (2.1 g, 0.015 mol, 3.0 eq). The mixture was stirred with heating at 90° C. for 1.5 hours. The reaction mixture was cooled to room temperature, and water (10 ml) was added. The mixture was extracted twice with ethyl acetate (30 ml). The organic layers were combined, washed with saturated brine (60 ml) and dried over anhydrous sodium sulfate. The drying agent was filtered off, and the filtrate was concentrated under reduced pressure to give (2-benzyloxyphenyl)acetonitrile (2.04 g, 100%) as a colorless solid. The reaction mixture was cooled to room temperature The mixture was extracted twice with ethyl acetate (30 ml) washed with saturated brine (60 ml) dried over anhydrous sodium sulfate The drying agent was filtered off the filtrate was concentrated under reduced pressure
来源 ID: ord-65b7b6d8a6394ec7a3867682c8823ee2PubChem References
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