反応 #4122617
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-2e950d53b7c74bea81083b15680e0703表示可能な構造データがありません
C1CC2C(=O)NCC1N2CC3=CC=CC=C3製品情報
8-benzyl-3,8-diazabicyclo[3.2.1]octan-2-one (CAS 824982-17-4) 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 21904723
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
12 反応 · 12 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2e950d53b7c74bea81083b15680e0703反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: The product of Example 1E (2.88 g, 13.3 mmol) in 40 mL THF was added via cannula to a mixture of LiAlH4 (1.52 g, 39.9 mmol) in 40 mL THF at 0° C. After the addition was complete, the reaction mixture was allowed to warm to ambient temperature and stir for 2 h. The mixture was warmed to reflux and stirred for 1 h. The reaction was cooled to 0° C. then 1.5 mL H2O, 1.5 mL 15% NaOH and 4.5 mL H2O were added sequentially to quench the reaction. The material was filtered, the residue was washed with EtOAc, and the filtrate was concentrated under reduced pressure and carried on directly to the next reaction. MS (DCl/NH3) m/z 203 (M+H)+. After the addition The mixture was warmed to reflux stirred for 1 h The reaction was cooled to 0° C. to quench the reaction The material was filtered the residue was washed with EtOAc the filtrate was concentrated under reduced pressure directly to the next reaction
ソース ID: ord-5e3812a945a54bb3a63331c3b8ade47e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: The product of Example 1E (2.88 g, 13.3 mmol) in 40 mL THF was added via cannula to a mixture of LiAlH4 (1.52 g, 39.9 mmol) in 40 mL THF at 0° C. After the addition was complete, the reaction mixture was allowed to warm to ambient temperature and stir for 2 h. The mixture was warmed to reflux and stirred for 1 h. The reaction was cooled to 0° C. then 1.5 mL H2O, 1.5 mL 15% NaOH and 4.5 mL H2O were added sequentially to quench the reaction. The material was filtered, the residue was washed with EtOAc, and the filtrate was concentrated under reduced pressure and carried on directly to the next reaction. MS (DCl/NH3) m/z 203 (M+H)+. After the addition The mixture was warmed to reflux stirred for 1 h The reaction was cooled to 0° C. to quench the reaction The material was filtered the residue was washed with EtOAc the filtrate was concentrated under reduced pressure directly to the next reaction
ソース ID: ord-5e3812a945a54bb3a63331c3b8ade47e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: The product of Example 1E (2.88 g, 13.3 mmol) in 40 mL THF was added via cannula to a mixture of LiAlH4 (1.52 g, 39.9 mmol) in 40 mL THF at 0° C. After the addition was complete, the reaction mixture was allowed to warm to ambient temperature and stir for 2 h. The mixture was warmed to reflux and stirred for 1 h. The reaction was cooled to 0° C. then 1.5 mL H2O, 1.5 mL 15% NaOH and 4.5 mL H2O were added sequentially to quench the reaction. The material was filtered, the residue was washed with EtOAc, and the filtrate was concentrated under reduced pressure and carried on directly to the next reaction. MS (DCl/NH3) m/z 203 (M+H)+. After the addition The mixture was warmed to reflux stirred for 1 h The reaction was cooled to 0° C. to quench the reaction The material was filtered the residue was washed with EtOAc the filtrate was concentrated under reduced pressure directly to the next reaction
ソース ID: ord-88cbf3f97e11468b9a6481d374e33262反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: The product of Example 1E (2.88 g, 13.3 mmol) in 40 mL THF was added via cannula to a mixture of LiAlH4 (1.52 g, 39.9 mmol) in 40 mL THF at 0° C. After the addition was complete, the reaction mixture was allowed to warm to ambient temperature and stir for 2 h. The mixture was warmed to reflux and stirred for 1 h. The reaction was cooled to 0° C. then 1.5 mL H2O, 1.5 mL 15% NaOH and 4.5 mL H2O were added sequentially to quench the reaction. The material was filtered, the residue was washed with EtOAc, and the filtrate was concentrated under reduced pressure and carried on directly to the next reaction. MS (DCl/NH3) m/z 203 (M+H)+. After the addition The mixture was warmed to reflux stirred for 1 h The reaction was cooled to 0° C. to quench the reaction The material was filtered the residue was washed with EtOAc the filtrate was concentrated under reduced pressure directly to the next reaction
ソース ID: ord-5e3812a945a54bb3a63331c3b8ade47e反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-2e950d53b7c74bea81083b15680e0703反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 8-Benzyl-3,8-diazabicyclo[3.2.1]octan-2-one (5.87 g, 27.1 mmol) in dry tetrahydrofuran (40 mL) was treated with 1M lithium aluminum hydride in THF (81.4 mL), heated at 60° C. for 2 hours, and then allowed to cool to room temperature and stir overnight. The mixture was cooled to 0° C. and treated in succession with water (4.4 mL), tetrahydrofuran (200 mL), 15% sodium hydroxide solution (4.4 mL), and water (13.3 mL). The mixture was filtered and the filter cake was rinsed with ethyl acetate. The filtrate was concentrated under reduced pressure to provide the title compound. MS (DCI/NH3) m/z: 203 (M+H)+. to cool to room temperature The mixture was cooled to 0° C. The mixture was filtered the filter cake was rinsed with ethyl acetate The filtrate was concentrated under reduced pressure
ソース ID: ord-6541db5665204de687e2c82f11ea6370反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Methyl 1-benzyl-5-(nitromethylene)-2-pyrrolidinecarboxylate (9.92 g, 35.9 mmol) and 5% platinum on activated carbon (11.25 g) were combined in methanol (100 mL) and shaken for 56 hours at ambient temperature under a hydrogen atmosphere (60 psi). The moisture was filtered and the filtrate concentrated to provide the title compound. MS (DCI/NH3) m/z: 217 (M+H)+. The moisture was filtered the filtrate concentrated
ソース ID: ord-61a470e5686246deb3f2b9c4ce994736反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 8-Benzyl-3,8-diazabicyclo[3.2.1]octan-2-one (5.87 g, 27.1 mmol) in dry tetrahydrofuran (40 mL) was treated with 1M lithium aluminum hydride in THF (81.4 mL), heated at 60° C. for 2 hours, and then allowed to cool to room temperature and stir overnight. The mixture was cooled to 0° C. and treated in succession with water (4.4 mL), tetrahydrofuran (200 mL), 15% sodium hydroxide solution (4.4 mL), and water (13.3 mL). The mixture was filtered and the filter cake was rinsed with ethyl acetate. The filtrate was concentrated under reduced pressure to provide the title compound. MS (DCI/NH3) m/z: 203 (M+H)+. to cool to room temperature The mixture was cooled to 0° C. The mixture was filtered the filter cake was rinsed with ethyl acetate The filtrate was concentrated under reduced pressure
ソース ID: ord-99769cc996174cbba9cee30a1da6e8ce反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Methyl 1-benzyl-5-(nitromethylene)-2-pyrrolidinecarboxylate (9.92 g, 35.9 mmol) and 5% platinum on activated carbon (11.25 g) were combined in methanol (100 mL) and shaken for 56 hours at ambient temperature under a hydrogen atmosphere (60 psi). The misture was filtered and the filtrate concentrated to provide the title compound. MS (DCI/NH3) m/z: 217 (M+H)+. The misture was filtered the filtrate concentrated
ソース ID: ord-b08555579183468dabae223e51a9e25f反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: The product of Example 1E (2.88 g, 13.3 mmol) in 40 mL THF was added via cannula to a mixture of LiAlH4 (1.52 g, 39.9 mmol) in 40 mL THF at 0° C. After the addition was complete, the reaction mixture was allowed to warm to ambient temperature and stir for 2 h. The mixture was warmed to reflux and stirred for 1 h. The reaction was cooled to 0° C. then 1.5 mL H2O, 1.5 mL 15% NaOH and 4.5 mL H2O were added sequentially to quench the reaction. The material was filtered, the residue was washed with EtOAc, and the filtrate was concentrated under reduced pressure and carried on directly to the next reaction. MS (DCl/NH3) m/z 203 (M+H)+. After the addition The mixture was warmed to reflux stirred for 1 h The reaction was cooled to 0° C. to quench the reaction The material was filtered the residue was washed with EtOAc the filtrate was concentrated under reduced pressure directly to the next reaction
ソース ID: ord-88cbf3f97e11468b9a6481d374e33262反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: The product of Example 1E (2.88 g, 13.3 mmol) in 40 mL THF was added via cannula to a mixture of LiAlH4 (1.52 g, 39.9 mmol) in 40 mL THF at 0° C. After the addition was complete, the reaction mixture was allowed to warm to ambient temperature and stir for 2 h. The mixture was warmed to reflux and stirred for 1 h. The reaction was cooled to 0° C. then 1.5 mL H2O, 1.5 mL 15% NaOH and 4.5 mL H2O were added sequentially to quench the reaction. The material was filtered, the residue was washed with EtOAc, and the filtrate was concentrated under reduced pressure and carried on directly to the next reaction. MS (DCl/NH3) m/z 203 (M+H)+. After the addition The mixture was warmed to reflux stirred for 1 h The reaction was cooled to 0° C. to quench the reaction The material was filtered the residue was washed with EtOAc the filtrate was concentrated under reduced pressure directly to the next reaction
ソース ID: ord-5e3812a945a54bb3a63331c3b8ade47ePubChem References
化合物の公開データベース記録に掲載された情報源です。
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