関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium sulfate decahydrate | HCID 62649 | — |
| 反応物 | 2-[(Piperidinocarbonyl)methyl]-8H-indeno[1,2-d]thiazole | HCID 18940973 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(2-piperidinoethyl)-8H-indeno[1,2-d]thiazole | HCID 18941102 | 25.2% |
反応手順
A solution of 500 mg of 2-[(piperidinocarbonyl)methyl]-8H-indeno[1,2-d]thiazole in 10 ml of tetrahydrofuran was added to a suspension of 160 mg of lithium aluminum hydride in 10 ml of tetrahydrofuran at 0° C., followed by heating under reflux for 1.5 hours. The reaction mixture was cooled to 0° C. again, and sodium sulfate decahydrate was added. The resulting mixture was stirred at room temperature for 30 minutes. After the insoluble matter was removed by filtration, the solvent was evaporated. The resulting oily substance was purified by silica gel column chromatography (eluent: chloroform:methanol=10:1), whereby 120 mg of 2-(2-piperidinoethyl)-8H-indeno[1,2-d]thiazole was obtained. Fumaric acid was added to the product in ethanol to cause crystallization, and the crystals were recrystallized to give a fumarate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05834499 |
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| 出典データセット | uspto-grants-1998_11 |
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| ORD ID | ord-5a0bc6916ef741158a495d4306794aa3 |
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| 出典メモ | uspto-grants-1998_11 |
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