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Hexane → [3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-4-yl]methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Sodium sulfate decahydrate | HCID 62649 | — |
| 反応物 | ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylate | HCID 9877977 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | [3-Methyl-1-(pyridin-2-yl)-1H-pyrazol-4-yl]methanol | HCID 23076503 | 92.7% |
反応手順
Lithium aluminium hydride (1.93 g) was added to a solution of ethyl 3-methyl-1-(2-pyridyl)-1H-pyrazole-4-carboxylate (15.00 g) in tetrahydrofuran (150 ml) at 0° C., and the mixture was stirred at room temperature for one hour. Sodium sulfate decahydrate (21.03 g) and hexane (100 ml) were added to the reaction mixture, and the mixture was stirred at room temperature for one hour. After the precipitate was removed by filtration, the filtrate was concentrated. The crystals obtained were collected by filtration to yield [3-methyl-1-(2-pyridyl)-1H-pyrazol-4-yl]methanol (11.38 g). This was recrystallized from acetone-hexane. Melting point: 116–117° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179823B1 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-f629b2eadfef435bb5d41732fed7d2f2 |
| 出典メモ | uspto-grants-2007_02 |