関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine chloride | HCID 24640 | — |
| 反応物 | 2-(4-Aminophenyl)benzothiazole | HCID 234475 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Benzenamine, 4-(2-benzothiazolyl)-2-iodo- | HCID 384526 | 71.4% |
反応手順
To a solution in acetic acid (35 ml) of 2-(4'-aminophenyl) benzothiazole (2.98 g, 0.0132 mol) prepared as above was added dropwise a solution of iodine monochloride (2.78 g, 0.0171 mol) in acetic acid (35 ml) over 10 minutes at room temperature, followed by stirring for 11/2 hours. After evaporation of the solvent, 60 ml dichloromethane was added to the residue and the resulting suspension was neutralised with sodium hydrogen carbonate. Then 300 ml of water was added. The organic layer was washed with 10% sodium hydrogen carbonate solution (150 ml), water (100 ml×2) and dried (mgSO4). The solvent was removed under reduced pressure, absorbed onto silica gel, and placed on top of a column of silica gel. Flash elution using ethyl acetate-hexane (2:5) yielded brown crystals (3.32 g, 69.6%), m.p. 143-144° 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-74a90100369d4fcf8789b0b766258894 |
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| 出典メモ | uspto-grants-2000_03 |
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