反应 #4063270
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-2dd64602e196462bbb20af7d7fca3793暂无可渲染的结构数据
CN(C)C(=O)C1CNCCO1产品信息
N,N-二甲基-2-吗啉羧胺(CAS 135072-23-0)的产品身份、结构标识及相关反应资料,供化学中间体检索、研发和采购评估使用。
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合成路线数据
6 条反应 · 6 篇文献
反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-2dd64602e196462bbb20af7d7fca3793反应条件: temp:0.00; pressure:0.00; stir:
来源 ID: ord-2dd64602e196462bbb20af7d7fca3793反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 1,3-dibromobenzene (387 μL, 3.20 mmol), N,N-dimethylmorpholine-2-carboxamide (506 mg, 3.20 mmol), Pd2(dba)3 (73.3 mg, 0.0800 mmol), rac-BINAP (154 mg, 0.240 mmol) and NaOtBu (369 mg, 3.84 mmol) in toluene (8 mL) was heated at 80° C. for 5 hours under nitrogen. After cooling to room temperature, the mixture was diluted with DCM and filtered through a Celite pad. The combined filtrate and washings were concentrated. The residue was purified by silica gel column chromatography (EtOAc/hexane=95:5→90:10→80:20→67:33→50:50) to afford desired product (424 mg, 42.3%) as orange oil. After cooling to room temperature filtered through a Celite pad The combined filtrate and washings were concentrated The residue was purified by silica gel column chromatography (EtOAc/hexane=95:5→90:10→80:20→67:33→50:50)
来源 ID: ord-55db98e3a3f64b9e8948c98a933c06fa反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4-benzyl-N,N-dimethylmorpholine-2-carboxamide (803 mg, 3.23 mmol), ammonium formate (2.15 g, 32.3 mmol) and 10% Pd/C (400 mg) in EtOH (20 mL) was heated at 50° C. for 1 hour. After cooling to room temperature, the catalyst was filtered off, washed with EtOH. The combined filtrate and washings were concentrated, and the residue was dissolved in EtOH (20 mL). Ammonium formate (2.15 g, 32.3 mmol) and 10% Pd/C (400 mg) were added to the mixture. The mixture was heated at 50° C. for 1 hour. After cooling to room temperature, the catalyst was filtered off, washed with EtOH. The combined filtrate and washings were concentrated to afford desired product (506 mg, 98.9%) as colorless oil. After cooling to room temperature the catalyst was filtered off washed with EtOH The combined filtrate and washings were concentrated the residue was dissolved in EtOH (20 mL) The mixture was heated at 50° C. for 1 hour After cooling to room temperature the catalyst was filtered off washed with EtOH The combined filtrate and washings were concentrated
来源 ID: ord-25c055a7a16c471fb048b310c0e74a8d反应条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 1,3-dibromobenzene (387 μL, 3.20 mmol), N,N-dimethylmorpholine-2-carboxamide (506 mg, 3.20 mmol), Pd2(dba)3 (73.3 mg, 0.0800 mmol), rac-BINAP (154 mg, 0.240 mmol) and NaOtBu (369 mg, 3.84 mmol) in toluene (8 mL) was heated at 80° C. for 5 hours under nitrogen. After cooling to room temperature, the mixture was diluted with DCM and filtered through a Celite pad. The combined filtrate and washings were concentrated. The residue was purified by silica gel column chromatography (EtOAc/hexane=95:5→90:10→80:20→67:33→50:50) to afford desired product (424 mg, 42.3%) as orange oil. After cooling to room temperature filtered through a Celite pad The combined filtrate and washings were concentrated The residue was purified by silica gel column chromatography (EtOAc/hexane=95:5→90:10→80:20→67:33→50:50)
来源 ID: ord-1f9d617b52674e358a1d6762263a57cf反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 4-benzyl-N,N-dimethylmorpholine-2-carboxamide (803 mg, 3.23 mmol), ammonium formate (2.15 g, 32.3 mmol) and 10% Pd/C (400 mg) in EtOH (20 mL) was heated at 50° C. for 1 hour. After cooling to room temperature, the catalyst was filtered off, washed with EtOH. The combined filtrate and washings were concentrated, and the residue was dissolved in EtOH (20 mL). Ammonium formate (2.15 g, 32.3 mmol) and 10% Pd/C (400 mg) were added to the mixture. The mixture was heated at 50° C. for 1 hour. After cooling to room temperature, the catalyst was filtered off, washed with EtOH. The combined filtrate and washings were concentrated to afford desired product (506 mg, 98.9%) as colorless oil. After cooling to room temperature the catalyst was filtered off washed with EtOH The combined filtrate and washings were concentrated the residue was dissolved in EtOH (20 mL) The mixture was heated at 50° C. for 1 hour After cooling to room temperature the catalyst was filtered off washed with EtOH The combined filtrate and washings were concentrated
来源 ID: ord-2b1248d825f548f289419b4b8f7641e9PubChem References
以下资料来自该化合物的公开数据库参考记录。
