反应 #4146938
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-87349322b22d430abb0d828557893844暂无可渲染的结构数据
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10 条反应 · 10 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-87349322b22d430abb0d828557893844反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-87349322b22d430abb0d828557893844反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4-methoxybenzylamine (1.37 g, 10 mmol) and acetone (0.81 mL, 11 mmol) in dry dichloroethane (20 mL) were stirred at room temperature for 30 minutes. To the solution was added sodium triacetoxyborohydride (3.18 g, 15 mmol) and the resulting mixture was stirred at room temperature for 17 hours. The reaction mixture was quenched with 1 N NaOH (50 mL) and the layers were separated. The aqueous layer was extracted with dichloromethane (2×20 mL). The combined extracts were washed with water (20 mL), brine (20 mL), dried over MgSO4, filtered through Celite, and concentrated under reduced pressure. The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine to provide 1.53 g of oil (85% yield). the resulting mixture was stirred at room temperature for 17 hours The reaction mixture was quenched with 1 N NaOH (50 mL) the layers were separated The aqueous layer was extracted with dichloromethane (2×20 mL) The combined extracts were washed with water (20 mL), brine (20 mL) dried over MgSO4 filtered through Celite concentrated under reduced pressure The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine
来源 ID: ord-c62e0636d08345dc90412128eeceef04反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 10A was prepared from a mixture of 1F and N-(4-methoxybenzyl)propan-2-amine following the procedure employed for the preparation of 1G. HPLC: Rt=4.27 min. (YMC S5 ODS 4.6×50 mm, 10-90% aqueous methanol containing 0.2% H3PO4, 4 min. gradient, monitored at 220 nm). MS (ES): m/z=356.1 [M+H]+.
来源 ID: ord-9848dcddd7fe4bc587540a60d6af9428反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 10A was prepared from a mixture of 1F and N-(4-methoxybenzyl)propan-2-amine following the procedure employed for the preparation of 1G. HPLC: Rt=4.27 min. (YMC S5 ODS 4.6×50 mm, 10-90% aqueous methanol containing 0.2% H3PO4, 4 min. gradient, monitored at 220 nm). MS (ES): m/z=356.1 [M+H]+.
来源 ID: ord-9848dcddd7fe4bc587540a60d6af9428反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4-methoxybenzylamine (1.37 g, 10 mmol) and acetone (0.81 mL, 11 mmol) in dry dichloroethane (20 mL) were stirred at room temperature for 30 minutes. To the solution was added sodium triacetoxyborohydride (3.18 g, 15 mmol) and the resulting mixture was stirred at room temperature for 17 hours. The reaction mixture was quenched with 1 N NaOH (50 mL) and the layers were separated. The aqueous layer was extracted with dichloromethane (2×20 mL). The combined extracts were washed with water (20 mL), brine (20 mL), dried over MgSO4, filtered through Celite, and concentrated under reduced pressure. The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine to provide 1.53 g of oil (85% yield). the resulting mixture was stirred at room temperature for 17 hours The reaction mixture was quenched with 1 N NaOH (50 mL) the layers were separated The aqueous layer was extracted with dichloromethane (2×20 mL) The combined extracts were washed with water (20 mL), brine (20 mL) dried over MgSO4 filtered through Celite concentrated under reduced pressure The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine
来源 ID: ord-f034f2c108064e789ffabbeaf39cc6a5反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4-methoxybenzylamine (1.37 g, 10 mmol) and acetone (0.81 mL, 11 mmol) in dry dichloroethane (20 mL) were stirred at room temperature for 30 minutes. To the solution was added sodium triacetoxyborohydride (3.18 g, 15 mmol) and the resulting mixture was stirred at room temperature for 17 hours. The reaction mixture was quenched with 1 N NaOH (50 mL) and the layers were separated. The aqueous layer was extracted with dichloromethane (2×20 mL). The combined extracts were washed with water (20 mL), brine (20 mL), dried over MgSO4, filtered through Celite, and concentrated under reduced pressure. The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine to provide 1.53 g of oil (85% yield). the resulting mixture was stirred at room temperature for 17 hours The reaction mixture was quenched with 1 N NaOH (50 mL) the layers were separated The aqueous layer was extracted with dichloromethane (2×20 mL) The combined extracts were washed with water (20 mL), brine (20 mL) dried over MgSO4 filtered through Celite concentrated under reduced pressure The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine
来源 ID: ord-89ad2147d0a54f0294f0c7e3279f16a0反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4-methoxybenzylamine (1.37 g, 10 mmol) and acetone (0.81 mL, 11 mmol) in dry dichloroethane (20 mL) were stirred at room temperature for 30 minutes. To the solution was added sodium triacetoxyborohydride (3.18 g, 15 mmol) and the resulting mixture was stirred at room temperature for 17 hours. The reaction mixture was quenched with 1 N NaOH (50 mL) and the layers were separated. The aqueous layer was extracted with dichloromethane (2×20 mL). The combined extracts were washed with water (20 mL), brine (20 mL), dried over MgSO4, filtered through Celite, and concentrated under reduced pressure. The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine to provide 1.53 g of oil (85% yield). the resulting mixture was stirred at room temperature for 17 hours The reaction mixture was quenched with 1 N NaOH (50 mL) the layers were separated The aqueous layer was extracted with dichloromethane (2×20 mL) The combined extracts were washed with water (20 mL), brine (20 mL) dried over MgSO4 filtered through Celite concentrated under reduced pressure The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine
来源 ID: ord-6d8ec897edc44632a1ed152717cdd70f反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4-methoxybenzylamine (1.37 g, 10 mmol) and acetone (0.81 mL, 11 mmol) in dry dichloroethane (20 mL) were stirred at room temperature for 30 minutes. To the solution was added sodium triacetoxyborohydride (3.18 g, 15 mmol) and the resulting mixture was stirred at room temperature for 17 hours. The reaction mixture was quenched with 1 N NaOH (50 mL) and the layers were separated. The aqueous layer was extracted with dichloromethane (2×20 mL). The combined extracts were washed with water (20 mL), brine (20 mL), dried over MgSO4, filtered through Celite, and concentrated under reduced pressure. The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine to provide 1.53 g of oil (85% yield). the resulting mixture was stirred at room temperature for 17 hours The reaction mixture was quenched with 1 N NaOH (50 mL) the layers were separated The aqueous layer was extracted with dichloromethane (2×20 mL) The combined extracts were washed with water (20 mL), brine (20 mL) dried over MgSO4 filtered through Celite concentrated under reduced pressure The residue was chromatographed eluting with 10% MeOH in dichloromethane with 1% triethylamine
来源 ID: ord-c62e0636d08345dc90412128eeceef04反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 10A was prepared from a mixture of 1F and N-(4-methoxybenzyl)propan-2-amine following the procedure employed for the preparation of 1G. HPLC: Rt=4.27 min. (YMC S5 ODS 4.6×50 mm, 10-90% aqueous methanol containing 0.2% H3PO4, 4 min. gradient, monitored at 220 nm). MS (ES): m/z=356.1 [M+H]+.
来源 ID: ord-9848dcddd7fe4bc587540a60d6af9428PubChem References
以下资料来自该化合物的公开数据库参考记录。
