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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 | 95% |
反応手順
To a solution of 114 g (447 mmol) of tert-butyl (3-bromophenyl)carbamate in 800 ml of DMF are added portionwise 19 g (475 mmol) of sodium hydride (60% in oil) 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-water and extracted with ethyl acetate. The organic phase is separated out by settling of the phases, dried over magnesium sulfate and evaporated. 115 g of tert-butyl (3-bromophenyl)-N-methylcarbamate are obtained in a yield of 95%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08129416B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-ba3433e1390b426396c07058c5da4ea4 |
| 出典メモ | uspto-grants-2012_03 |