関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Methylpyridine | HCID 7975 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Chlorosulfonic acid | HCID 24638 | — |
| 反応物 | Benzenamine, 4-(2-benzothiazolyl)-2-iodo- | HCID 384526 | — |
| 生成物 | Sodium 4-(benzothiazol-2-yl)phenylsulphamate | HCID 23717892 | — |
反応手順
To anhydrous 2-picoline (1.05 g, 11 mmol) was slowly added dropwise chlorsulphonic acid (0.26 g, 2.21 mmol) below 10° C. then 2-(4'-amino-3'-iodophenyl)benzothiazole (0.5 g, 2.21 mmol). The mixture was heated to 50° C. with stirring for 1 hour. After leaving to stand for 2 hours at room temperature, 6 ml of 10% aqueous sodium carbonate was added. The resulting mixture was stirred for 40 minutes at room temperature and concentrated under reduced pressure. The precipitate was filtered off, washed carefully with cold water and treated with hot chlorform. Golden crystals were afforded (0.62 g, 85.5%), m.p. 288-290° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06034246 |
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| 出典データセット | uspto-grants-2000_03 |
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| ORD ID | ord-238ae6d3d5b64f388881ec0f478e52b2 |
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| 出典メモ | uspto-grants-2000_03 |
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