反応 #4063270
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-2dd64602e196462bbb20af7d7fca3793表示可能な構造データがありません
CN(C)C(=O)C1CNCCO1製品情報
N,N-dimethylmorpholine-2-carboxamide (CAS 135072-23-0) 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 20472122
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-2dd64602e196462bbb20af7d7fca3793反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2dd64602e196462bbb20af7d7fca3793反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 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)
ソース ID: ord-55db98e3a3f64b9e8948c98a933c06fa反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 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
ソース ID: ord-25c055a7a16c471fb048b310c0e74a8d反応条件: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 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)
ソース ID: ord-1f9d617b52674e358a1d6762263a57cf反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 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
ソース ID: ord-2b1248d825f548f289419b4b8f7641e9PubChem References
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