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Acetic Anhydride → N-(7-bromobenzo[d]thiazol-2-yl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 2-Benzothiazolamine, 6-bromo- | HCID 85149 | — |
| 反応物 | N-(6-bromo-1,3-benzothiazol-2-yl)acetamide | HCID 3240669 | — |
| 反応物 | 7-Bromo-1,3-benzothiazol-2-amine | HCID 20357112 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(7-bromobenzo[d]thiazol-2-yl)acetamide | HCID 57584914 | 72% |
反応手順
The mixture (1.02 g, 4.45 mmol) of 7-bromobenzo[d]thiazol-2-amine and 6-bromobenzo[d]thiazol-2-amine and DMAP (620.6 mg, 5.079 mmol) were suspended in DCM (40 mL) and acetic anhydride (0.46 mL, 4.9 mmol) was added. The reaction was stirred under nitrogen at RT for 2 hours and was then quenched with 1 N HCl (25 mL). The layers were separated, and the aqueous phase was extracted with DCM, and the organic extracts were washed with 1 N HCl, dried over sodium sulfate, filtered, and concentrated to provide the mixture (865 mg, 72% yield) of N-(7-bromobenzo[d]thiazol-2-yl)acetamide and N-(6-bromobenzo[d]thiazol-2-yl)acetamide. MS (ESI pos. ion) m/z: 271 (MH+, 79Br), 273 (MH+, 81Br). Calculated exact mass for C9H7BrN2S: 270 (79Br), 272 (81Br).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07928140B2 |
| 出典データセット | uspto-grants-2011_04 |
| ORD ID | ord-676de2c98c8446698854ab6e1ba52e74 |
| 出典メモ | uspto-grants-2011_04 |