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Sodium Thiosulfate → 4-Bromo-5-fluoro-2-methylaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 5-Fluoro-o-toluidine | HCID 67774 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Bromo-5-fluoro-2-methylaniline | HCID 7018044 | 102.1% |
反応手順
To a solution of 49.0 g of 5-fluoro-o-toluidine in 600 mL of dichloromethane was added 69.7 g of N-bromosuccinimide at 0° C., and stirred at this temperature for an hour. Then sodium thiosulfate aqueous solution was added, and the reaction solution was evaporated and diluted with ethyl acetate. The organic layer was washed successively with water and saturated brine and dried over anhydrous magnesium sulfate. Then the solvent was evaporated, and the precipitated crystals were washed with diethyl ether:n-hexane=1:10, to afford 81.6 g of the title compound as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429609B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-569024928a0c4303b8725395bd1d2d18 |
| 出典メモ | uspto-grants-2008_09 |