関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Amino-5-(diethylamino)toluene | HCID 67364 | — |
| 反応物 | N,N-Diethyltoluene-2,5-diamine hydrochloride | HCID 108623 | — |
| 反応物 | 4-Hydroxy-6-fluorophenanthridine | HCID 54165240 | — |
| 触媒 | Silver Nitrate | HCID 24470 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl acetate hexane | HCID 21226206 | 27.1% |
反応手順
While stirring a mixture comprising 59 mg of 4-hydroxy-6-fluorophenanthridine, 85 mg of 2-amino-5-diethylaminotoluene hydrochroride (21) and 4 ml of ethanol at 20° C., a solution comprising 258 mg of silver nitrate dissolved in 0.8 ml of water was added thereto drop-by-drop. Next, with 0.84 ml of 25% ammonia solution added, reaction was allowed to proceed at 20° C. for a period of 24 hr. After the completion of the reaction, the reacted solution was introduced into water. After extraction by chloroform, the extract was concentrated. After purification by column chromatography, 29 mg of indoaniline described in the exemplified compound 3-131 was obtained as deep blue crystal on recrystallization from hexane-ethyl acetate solvent (yield 27.1%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05892042 |
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| 出典データセット | uspto-grants-1999_04 |
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| ORD ID | ord-f57489be2c9e4ddf9f1b244268d0d499 |
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| 出典メモ | uspto-grants-1999_04 |
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