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Methyl iodide → N-BOC-N-Methyl-3-bromoaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | N-(tert-Butoxycarbonyl)-3-bromoaniline | HCID 2757254 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-BOC-N-Methyl-3-bromoaniline | HCID 22997148 | 113.4% |
反応手順
To a solution of 128 g (470 mmol) of tert-butyl 3-bromophenylcarbamate in 800 mL of dimethylformamide, 19 g (475 mmol) of sodium hydride (60% in oil) are added portionwise and the reaction medium is stirred until the evolution of gas has ceased. 29.3 mL (470 mmol) of methyl iodide are added dropwise and stirring is continued for 18 hours. The reaction medium is poured into ice-cold water and extracted with ethyl acetate. The organic phase is separated out after settling of the phases, dried over magnesium sulfate and evaporated. 152.5 g (92%) of tert-butyl 3-bromophenyl-N-methylcarbamate are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383652B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-86a40377e43d4f53830c5f2b55ca051d |
| 出典メモ | uspto-grants-2013_02 |