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Triethylamine → 2-((2,4-Dichlorobenzyl)(methyl)amino)-1-(3-nitrophenyl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Bromo-1-(3-nitrophenyl)ethan-1-one | HCID 75213 | — |
| 反応物 | Benzenemethanamine, 2,4-dichloro-N-methyl- | HCID 485424 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-((2,4-Dichlorobenzyl)(methyl)amino)-1-(3-nitrophenyl)ethanone | HCID 67455430 | — |
反応手順
Into a 100-mL 3-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of 2-bromo-1-(3-nitrophenyl)ethanone (2 g, 8.23 mmol, 1.00 equiv), triethylamine (3.4 g, 4.00 equiv), (2,4-dichlorophenyl)-N-methylmethanamine (1.9 g, 10.05 mmol, 1.20 equiv), 1,4-dioxane (50 mL). The resulting solution was stirred for 2 h at room temperature at which time it was judged to be complete by LCMS. The mixture was concentrated under vacuum and the residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:100-1:50). This resulted in 1.5 g (50%) of 2-((2,4-dichlorobenzyl)(methyl)amino)-1-(3-nitrophenyl)ethanone as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541448B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-498c0b3df70745599d9601905ee71632 |
| 出典メモ | uspto-grants-2013_09 |