関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydride | HCID 166653 | — |
| 反応物 | ethyl 1-(2-propynyl)-3-trifluoromethyl-1H-pyrrole-4-carboxylate | HCID 14370787 | — |
| 反応物 | Potassium alloy, nonbase, K,Na | HCID 16211683 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(2-propynyl)-3-trifluoromethyl-1H-pyrrole-4-methanol | HCID 14370788 | 54.6% |
反応手順
At 0° C., 1.95 g of lithium aluminium hydride were introduced in small portions into a solution of 12.6 g of ethyl 1-(2-propynyl)-3-trifluoromethyl-1H-pyrrole-4-carboxylate in 65 ml of tetrahydrofuran with stirring for 2 hours at 20° C. 10 ml of ethyl acetate were added to eliminate possible excess of hydride and the reaction mixture was poured into a saturated solution of sodium-potassium double tartrate. After extraction with ethyl acetate, the extracts were concentrated to dryness by distillation under reduced pressure. The residue was chromatographed over silica and eluted with a mixture of hexane and ethyl acetate (7-3) to obtain 5.7 g of 1-(2-propynyl)-3-trifluoromethyl-1H-pyrrole-4-methanol melting at 45° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04737513 |
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| 出典データセット | uspto-grants-1988_04 |
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| ORD ID | ord-bf7b0a646c1546ba9e56014f1a85bc9f |
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| 出典メモ | uspto-grants-1988_04 |
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