関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | p-Tolylthiourea | HCID 722833 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Amino-6-methylbenzothiazole | HCID 17335 | 67% |
反応手順
(4-Methylphenyl)thiourea (2 mmol) was added to AcOH (4 ml), and the suspension was heated to 80° C. To the solution formed was added 33% HBr in AcOH (4 mmol) followed by DMSO (2.1 mmol). After stirring at 80° C. for 1 h, the reaction mixture was cooled to 50° C., diluted with EtOAc (10 ml) and filtered. The product (as HBr-salt) was taken up in H2O (5 ml) and treated with 1M aq. NaHCO3 (2 ml). Stirring was continued for 0.2 h. The precipitated aminobenzothiazole was then filtered, washed with H2O (10 ml) and dried (16 h at 45° C./20 mb); yield 67%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087761B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-2c38c04a2ff54f61871a1c6ab0095848 |
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| 出典メモ | uspto-grants-2006_08 |
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