関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | 3-Hydroxy-3-methyl-2-butanone | HCID 8261 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3H-Indole, 2,3,3-trimethyl- | HCID 15427 | — |
反応手順
408 parts of 2-methyl-2-hydroxy-butan-3-one, 558 parts of aniline and 20 parts of acetic acid in 650 parts of toluene are heated, with removal of water from the system, until no more water separates off. The volatile constituents are then distilled off until the internal temperature reaches 220° C. The distillate can be re-used, without further treatment, in a subsequent batch. The residue is kept for 5 hours at 220° C. and is then cooled to 160° C., and 40 parts of concentrated hydrochloric acid are added. After heating for a further three hours, during which the water formed distils off, the reaction is complete. The product is either directly processed further or distilled. 498 parts of 2,3,3-trimethyl-indolenine are obtained, corresponding to 78.5% of theory, based on 2-methyl-2-hydroxy-butan-3-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04255333 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-f55916a9d946457c97c38bbdf82d6a8e |
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| 出典メモ | uspto-grants-1981_03 |
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