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N-bromobutanimide → N-(5-bromo-4-chloropyridin-2-yl)-2,2-dimethylpropanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | N-(4-Chloropyridin-2-yl)pivalamide | HCID 10656204 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-(5-bromo-4-chloropyridin-2-yl)-2,2-dimethylpropanamide | HCID 59613421 | 66.4% |
反応手順
NBS (8.37 g. 47.0 mmol) was added to a solution of N-(4-chloropyridin-2-yl)pivalamide (2.00 g, 9.40 mmol) in dry acetonitrile (20 mL). The resulting suspension was heated for 3 hr and then cooled to r.t. The solvent was removed in vacuo and the crude mixture was diluted with ethyl acetate (100 mL). The organic phase was washed with aqueous NaOH (10%, 2×40 mL), water (40 mL) and dried (MgSO4). The solvent was removed in vacuo and the crude mixture was purified by flash chromatography on silica, eluting with ethyl acetate and hexane (1/9), to give the title compound as a colourless solid (1.82 g, 66%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367658B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-a0fce03ae79e4e8882d8fa7ee697e6d1 |
| 出典メモ | uspto-grants-2013_02 |