関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2,3-Difluorobenzoyl chloride | HCID 519549 | — |
| 反応物 | N2-(tert-Butyl)pyridine-2,3-diamine | HCID 15656135 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-(tert-butylamino)pyridin-3-yl)-2,3-difluorobenzamide | HCID 59003070 | — |
反応手順
To a solution of N2-tert-butylpyridine-2,3-diamine in dry DCM (150 mL) was added DIEA (17 mL, 95.5 mmol). The solution was cooled to 0° C. and carefully added 2,3-difluorobenzoyl chloride (8.35 g, 47.30 mmol). The reaction was allowed to warm up to RT and stirred for 1 hr. The mixture was then washed with water, saturated NaHCO3, and dried over MgSO4. Removal of the solvent by evaporation, the residue was purified by silica gel chromatography (5%-60% EtOAc/hexane) to yield N-(2-(tert-butylamino)pyridin-3-yl)-2,3-difluorobenzamide (4.0 g, 13.10 mmol); LC-MS m/e=306.1 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07872031B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-ef7d54834db9401fa8d9e04131ed7fd6 |
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| 出典メモ | uspto-grants-2011_01 |
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