関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbazole | HCID 6854 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 3-(1-Acetyl-4-piperidinyl)propionyl chloride | HCID 10465951 | — |
| 溶媒 | Nitromethane | HCID 6375 | — |
| 生成物 | 1-(3-Carbazolyl)-3-(1-acetylpiperidin-4-yl)-1-propanone | HCID 21476712 | 25% |
反応手順
To a 90 ml solution of 5.0 g of carbazole and 7.2 g of 3-(1-acetylpiperidin-4-yl)propionyl chloride in nitromethane, 9.3 g of aluminum chloride was added little by little, followed by stirring at 70° C. for 11 hours. The reaction mixture was poured over 100 ml of ice water, and the organic layer was separated and then washed by sequential additions of a 50 ml saturated aqueous sodium hydrogen carbonate solution and 50 ml of distilled water. After the mixture was dried over anhydrous sodium sulfate, the solvent was distilled off to yield an oily residue. The residue was purified by silica gel column chromatography (developing solvent: ethyl acetate-methanol=20:1 (v/v)) to yield 2.6 g of the title compound as a light yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05527800 |
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| 出典データセット | uspto-grants-1996_06 |
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| ORD ID | ord-d0e0290264c64ebfb3fed5b936f94e58 |
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| 出典メモ | uspto-grants-1996_06 |
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