関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | (3,5-Difluorophenyl)thiourea | HCID 2783293 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 5,7-Difluorobenzo[d]thiazol-2-amine | HCID 15050564 | 90.7% |
反応手順
To a suspension of N-(3,5-difluorophenyl) thiourea (3.40 g, 18.07 mmol) in DCE (95 mL) was added a solution of bromine in DCE (5 mL) below 30° C. The mixture was heated at reflux for 2.5 h, then cooled to 10° C., and the precipitate formed was collected by filtration and washed with DCE. The solid was stirred with water (200 mL), basified by treatment with conc. ammonium hydroxide, filtered, and dried in a vacuum oven to afford 5,7-difluoro-1,3-benzothiazol-2-amine (3.05 g, 90%). ret. time 2.18; m/z 187.1 (MH+) 1H NMR (400 MHz, DMSO-d6) δ 6.92 (m, 1H), 7.00 (m, 2H), 7.92 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08013166B2 |
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| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-cff82a0362244790a89eafa798a1505e |
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| 出典メモ | uspto-grants-2011_09 |
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