関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Methyl 6-chloropyridazine-3-carboxylate | HCID 12379801 | — |
| 反応物 | diisobutylaluminium hydride THF | HCID 86597605 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (6-Chloropyridazin-3-yl)methanol | HCID 20557609 | 12.2% |
反応手順
In tetrahydrofuran (100 mL) was dissolved methyl 6-chloropyridazin-3-carboxylate (1.726 g), the solution was cooled to 0° C., 1M diisobutyaluminum hydride-tetrahydrofuran solution (20 mL) was added dropwise to the solution, and the mixture was stirred at the same temperature for 20 minutes. To the reaction mixture were successively added water (10 mL) and 1N hydrochloric acid (20 mL) at 0° C. After adding a saturated aqueous sodium bicarbonate solution to the mixture at room temperature, the mixture was extracted with chloroform. The extract was dried over anhydrous sodium sulfate, and the residue obtained by concentrating the extract under reduced pressure was purified by silica gel column chromatography (n-hexane:ethyl acetate=90:10 to 25:75) to obtain (6-chloropyridazin-3-yl)methanol (177 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09302996B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-386545005abc476c9ae7e4494f3e243d |
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| 出典メモ | uspto-grants-2016_04 |
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