関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Cyano-6-methoxy benzothiazole | HCID 342109 | — |
| 反応物 | Pyridinium hydrochloride | HCID 21584435 | — |
| 生成物 | 2-Cyano-6-hydroxybenzothiazole | HCID 9881912 | 45% |
反応手順
A mixture of 6-methoxybenzo[d]thiazole-2-carbonitrile (1.0 g, 5.3 mmol) and dry pyridinium hydrochloride (11.3 g, 98.1 mmol) was stirred at 190° C. for 3 h. After the completion of reaction, it was cooled to room temperature to obtain a yellow solid. This solid was purified by flash chromatography (silica gel, methylene chloride/ethyl acetate=25/1) to afford 6-hydroxybenzo[d]thiazole-2-carbonitrile as a yellow solid (0.42 g, 45%). 1H-NMR (DMSO-d6, 300 MHz): δ 10.20 (s, 1H), 8.70 (m, 1H), 8.45 (m, 1H), 8.10 (m, 1H) ppm; MS (ESI): 177.1 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09353111B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-ebebb1a802a44e6fa528c96d4fd79f62 |
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| 出典メモ | uspto-grants-2016_05 |
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