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Bromine → 2-Amino-6-(4-fluorophenoxy)benzothiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Benzenamine, 4-(4-fluorophenoxy)- | HCID 147633 | — |
| 反応物 | Potassium thiocyanate | HCID 516872 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Amino-6-(4-fluorophenoxy)benzothiazole | HCID 21985512 | 103.2% |
反応手順
A solution of 4-(4′-fluorophenoxy)aniline (0.305 g, 1.50 mmol) and KSCN (0.29 g, 3.00 mmol, 2.0 eq) in 3 mL acetic acid was cooled at about 5° C., and was treated dropwise with a solution of bromine (0.077 mL, 1.50 mmol, 1.0 eq) in 2 mL acetic acid. The mixture was stirred at room temperature for about 2 hours. The precipitate was filtered off and washed with Et2O. The mother liquid from the filtration was concentrated, and the residue was combined with the precipitate. The obtained solid was neutralized with saturated sodium carbonate solution, and a new precipitate was formed. It was filtered off, washed with water, and dried under vacuum to give the desired compound 0.403 g (90%). LC/MS 261.2 (M+1); LC retention time 2.44 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091227B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-39cabe140ee74440b053a8e259355b3d |
| 出典メモ | uspto-grants-2006_08 |