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Trifluoroacetic acid → 3-Bromo-N-methylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | N-BOC-N-Methyl-3-bromoaniline | HCID 22997148 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Bromo-N-methylaniline | HCID 7018299 | 90.6% |
反応手順
3.6 g (12.7 mmol) of tert-butyl (3-bromophenyl)-N-methylcarbamate, prepared in a manner analogous to Example 1b), are dissolved in 15 ml of dichloromethane. 5 ml of trifluoroacetic acid are added and the reaction mixture is stirred at ambient temperature for 1 hour. The reaction is halted by the addition of 50 ml of a saturated sodium hydrogencarbonate solution and then extraction is carried out with ethyl acetate. The organic phases are combined and dried over sodium sulfate. The solvents are evaporated and then the residue is chromatographed on silica gel (heptane/ethyl acetate 50/50). 2.14 g of 3-bromo-N-methylaniline are obtained in the form of an oil. Yield=90%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07626054B2 |
| 出典データセット | uspto-grants-2009_12 |
| ORD ID | ord-c24b085d45fe4a24b8a82edbe47772a9 |
| 出典メモ | uspto-grants-2009_12 |