関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Aminobenzophenone | HCID 14346 | — |
| 反応物 | Hydrogen iodide | HCID 24841 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 4-Iodobenzophenone | HCID 569638 | — |
反応手順
A solution of 57% aqueous HI (3.29 ml, 25 mmol) dissolved in DMSO (25 ml) was added dropwise to a solution of 4-aminobenzophenone (0.986 g, 5 mmol) in a mixture of 25 ml of DMSO and KNO2 (0.851 g, 10 mmol) at 35° C. with agitation. The added mixture was stirred at 35° C. for 10 minutes and then was transferred to a solution containing K2CO3 (5 g) in 100 ml ice-water. The reaction mixture was then taken up in ether, and then the ethereal extracts were washed with water and dried over anhydrous magnesium sulfate. Removal of the solvent under reduced pressure gave the crude 4-iodobenzophenone. The crude product was further purified by column chromatography to obtain 4-iodobenzophenone. The yield determined by gas chromatography was 88% (based on decane as an internal standard).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06943257B2 |
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| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-7a59f78b3b53467ba4027ed25d36eaab |
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| 出典メモ | uspto-grants-2005_09 |
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