関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Mucobromic Acid | HCID 3033972 | — |
| 反応物 | Aniline ethanol | HCID 22137766 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178419561 | HCID 178419561 | — |
反応手順
The procedure as disclosed in the literature (Simonis, H. Ber. Deut. Chem. Ges. 1901, 34, 509; U.S. Pat. No. 6,747,159) is used. 3.54 g of aniline are dissolved in 15 ml of ethanol in a 100 ml beaker. Separately, 5 g of mucobromic acid are dissolved in 15 ml of ethanol in a 100 ml Erlenmeyer flask. This solution is added dropwise to the aniline/ethanol solution, with cooling. The reaction mixture turns immediately yellow, then orange, with development of CO2. At the end of the addition, the mixture is heated in a water bath until its volume is reduced by one half. The resulting solution is cooled with an ice-salt mixture, forming a yellow crystalline precipitate. This solid is collected on a fritted glass filter to afford pure product 5; additional product 5 can be recovered from concentration and recrystallization of the mother liquor.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481752B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-880d2b139b6e475a940ad403434b4ca6 |
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| 出典メモ | uspto-grants-2013_07 |
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