関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Methyl 3-thioureidobenzoate | HCID 726316 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Methyl 2-aminobenzo[d]thiazole-7-carboxylate | HCID 10910742 | — |
反応手順
At 0° C. a solution of bromine (13.4 mmol) in acetic acid (9.4 mL) is added dropwise to a vigorously stirred solution of 3-thioureido-benzoic acid methyl ester (12.5 ml) in acetic acid (37 mL). The mixture is allowed to reach RT, stirred at 70° C. for 4 h and cooled to RT. Ether is added and the precipitate is filtered off. The residue is stirred vigorously in a sat aq. NaHCO3 solution, filtered off and washed with water. The obtained solid is dried in vacuo to give the desired product which is used without further purification. LC-MS: tR=0.62 min; [M+H]+=209.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08063099B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-736c1d15207d4c61b9c0d300624b870c |
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| 出典メモ | uspto-grants-2011_11 |
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