関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 5-Fluoro-2-methylbenzothiazole | HCID 597437 | — |
| 溶媒 | Ethylene Glycol | HCID 174 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 2-Amino-4-fluorobenzene-1-thiol | HCID 11105480 | — |
反応手順
A solution of 5-fluoro-2-methylbenzo[d]thiazole (1.2 g, 7.18 mmol) in ethylene glycol and NaOH (5N, 2 ml) was degassed under N2 for 10 min, then refluxed at 129° C. for 3 hours. The solution was cooled to 0° C. and then acidified to pH 3˜4 using c. HCl. The mixture was extracted with EtOAc (2×50 ml). The organic layer was washed with brine and dried with Na2SO4 and concentrated in vacuo. The crude residue (1.01 g, 98%) was used directly in the next step without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09328067B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-017153fa48f5499ca9f2d74947ca74d0 |
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| 出典メモ | uspto-grants-2016_05 |
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