関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-(Chloromethyl)benzothiazole | HCID 304978 | — |
| 反応物 | HCID 22998605 | HCID 22998605 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(2-Benzothiazolyl)methoxy-2-piperidinomethyltetralin Hydrochloride | HCID 22998531 | 50.6% |
反応手順
To a solution of 6-hydroxy-2-piperidinomethyltetralin hydrochloride (205 mg, Reference Example 19) and 2-chloromethylbenzothiazole (183 mg) in DMF (10 ml) was added potassium carbonate (327 mg) and the reaction mixture was stirred at room temperature for 4 days and further at 60° C. for 7 hr. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, dried, and concentrated. The residue was purified by silica gel column chromatography (eluent: ethyl acetate: methanol=10:1), alumina column chromatography (eluent: ethyl acetate: hexane=1:4) and converted into its hydrochloride, which was recrystallized from methanol-ethyl acetate to obtain the titled compound (158 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06613805B2 |
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| 出典データセット | uspto-grants-2003_09 |
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| ORD ID | ord-77b21899d388493abc2cd7dfec291e7e |
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| 出典メモ | uspto-grants-2003_09 |
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