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Dabco → 3-chloro-4-fluoro-N-pyrimidin-4-ylbenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | 4-Aminopyrimidine | HCID 68958 | — |
| 反応物 | 3-Chloro-4-fluorobenzenesulphonyl chloride | HCID 145222 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-chloro-4-fluoro-N-pyrimidin-4-ylbenzenesulfonamide | HCID 59436491 | 27% |
反応手順
4-Aminopyrimidine (1.0 g, 10.5 mmol) and DABCO™ (1.18 g, 10.5 mmol) were added concurrently to a solution of 3-chloro-4-fluorobenzenesulfonyl chloride (1.25 mL, 10.0 mmol) in anhydrous acetonitrile (49 mL). The reaction mixture immediately turned yellow and a precipitate was formed. After stirring for 16 hours, the mixture was concentrated in vacuo. The crude material was suspended in ethyl acetate (75 mL) and water (75 mL) and stirred for 15 minutes. The resulting solid was filtered and dried in vacuo to afford the title compound, 0.83 g, 27% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541588B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-257ca3bd31f446f79a741ae7a987f53f |
| 出典メモ | uspto-grants-2013_09 |