関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,3,5-Triiodobenzoic acid | HCID 6948 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,3,5-Triiodobenzoyl chloride | HCID 2760806 | — |
反応手順
A mixture of 15.0 g (30.0 mmol) of 2,3,5-triiodobenzoic acid and 19.0 g (150 mmol) of oxalyl chloride in 60 ml of dry dichloromethane was placed under nitrogen and cooled to 0° C. Two drops of dry DMF were added, the ice bath was removed and the resulting suspension was stirred at room temperature for 1.5 hrs. The resulting brown solution was concentrated in vacuo to produce a tan solid. The solid was dissolved in 30 ml of dry toluene and was concentrated in vacuo. The toluene concentration was repeated two more times to yield 2,3,5-triiodobenzoyl chloride as a tan solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05484585 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-1597f145b8304576ab4ccfc670b2f5fc |
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| 出典メモ | uspto-grants-1996_01 |
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