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Bromoacetyl bromide → 2-(Bromoacetyl)amino-N-(5-chloropyridin-2-yl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromoacetyl bromide | HCID 61147 | — |
| 反応物 | 2-amino-N-(5-chloropyridin-2-yl)benzamide | HCID 21906381 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Diisopropylethylamine | HCID 81531 | — |
| 生成物 | 2-(Bromoacetyl)amino-N-(5-chloropyridin-2-yl)benzamide | HCID 21906359 | 89.6% |
反応手順
To a stirred solution of 2-amino-N-(5-chloropyridin-2-yl)benzamide (1.65 g, 6.66 mmol) in tetrahydrofuran (60 mL) and diisopropylethyl amine (1.28 mL) was added bromoacetyl bromide (0.64 mL, 7.32 mmol) dropwise at 0° C. The reaction mixture was warmed to room temperature and stirred overnight. Diluted the reaction mixture with ethyl acetate (120 mL) and water (50 mL). Separated the organic layer and washed with water (25 mL), saturated sodium bicarbonate (50 mL), 0.2 N hydrochloric acid (25 mL), water (50 mL). Dried over sodium sulfate and remove the solvent to get crude product (2.2 g), which was used as such in the following step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129245B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-053255370c4843838465b713191e6951 |
| 出典メモ | uspto-grants-2006_10 |