関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 1H-Indole, 1-ethyl-2-methyl- | HCID 170432 | — |
| 反応物 | Ammonia hydroxide | HCID 21862953 | — |
| 反応物 | 2,4-Bis(1-n-propyl-2-methyl-3-indolyl)-4-oxobutanoic acid | HCID 54110624 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 54027974 | HCID 54027974 | — |
反応手順
A stirred mixture of 7.0 g (0.0157 mole) of the 2,4-bis(1-n-propyl-2-methyl-3-indolyl)-4-oxobutanoic acid prepared as described in A above, 2.7 g (0.017 mole) of 1-ethyl-2-methylindole, 100 ml of acetic anhydride and 1.0 ml of glacial acetic acid was aerated by bubbling air through the mixture for approximately eight hours at a temperature in the range of 48°-52° C. The solid that formed was collected by filtration. A second crop of product was obtained by drowning the filtrate in a stirred mixture of ice, benzene and sufficient concentrated ammonia hydroxide to make the mixture slightly alkaline. The benzene layer was separated, dried over molecular sieves, filtered and the filtrate set aside for several hours. The crystals, which separated from the solution, were collected by filtration and combined with the first crop of product. The combined solids were dried in vacuo at 60° C. to obtain 3,5-bis-(1-n-propyl-2-methyl-3-indolyl)-5-(1-ethyl-2-methyl-3-indolyl)-2(5H)-furanone (Formula III: R=CH3CH2CH2 ; R1 =R3 =CH3 ; R2 =CH3CH2 ; Y=Y1 =H) as a tan solid which decomposed at 179° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04377698 |
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| 出典データセット | uspto-grants-1983_03 |
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| ORD ID | ord-7bd25bf9b0594b448fc828ef88520bd6 |
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| 出典メモ | uspto-grants-1983_03 |
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