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Hydrochloric Acid → N-((6-chloropyridin-3-yl)methyl)-N-ethyl-2-methyl-4-nitro-8-oxa-2-aza-bicyclo[3.2.1]oct-3-en-3-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Butanedial | HCID 12524 | — |
| 反応物 | N-((6-Chloro-3-pyridinyl)methyl)-N-ethyl-N'-methyl-2-nitro-1,1-ethenediamine | HCID 86457 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-((6-chloropyridin-3-yl)methyl)-N-ethyl-2-methyl-4-nitro-8-oxa-2-aza-bicyclo[3.2.1]oct-3-en-3-amine | HCID 58496253 | 40% |
反応手順
To a 50 ml round bottom flask was added 1.35 g (0.005 mol) N-((6-chloropyridin-3-yl)methyl)-N-ethyl-N′-methyl-2-nitroethene-1,1-diamine, 30 ml dry acetonitrile, 0.860 g (0.01 mol) succinaldehyde and catalytic concentrated HCl. The reaction was stirred at r.t. and monitored by TLC. After completion, the mixture was evaporated to remove solvent and purified by column chromatography to afford final product as faint yellow powder with 40% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08563546B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-91bba571e5844645b9cdff758538430c |
| 出典メモ | uspto-grants-2013_10 |