関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | N,N-Diethyltoluene-2,5-diamine hydrochloride | HCID 108623 | — |
| 反応物 | Phenanthridin-4-ol | HCID 22625105 | — |
| 触媒 | Silver Nitrate | HCID 24470 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl acetate hexane | HCID 21226206 | 35.1% |
反応手順
A mixture comprising 390 mg of 4-hydroxyphenanthridine (13), 430 mg of 2-amino-5-diethylaminotoluene hydrochloride (21) and 15 ml of ethanol was stirred at 20° C. and a solution comprising 1.02 g of silver nitrate dissolved in 4.5 ml of water was added thereto drop-by-drop. Then, 1.7 ml of 25% ammonia solution was added and the 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 ethyl acetate, the extract was concentrated. After purification by column chromatography, 259 mg of deep blue crystal of indoaniline (22) was obtained on recrystallization by hexane-ethyl acetate (yield 35.1%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05792863 |
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| 出典データセット | uspto-grants-1998_08 |
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| ORD ID | ord-d64100bd7a7443fc8b02c3cf82910eff |
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| 出典メモ | uspto-grants-1998_08 |
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