참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydride | HCID 166653 | — |
| 반응물 | ethyl 1-(2-propynyl)-3-trifluoromethyl-1H-pyrrole-4-carboxylate | HCID 14370787 | — |
| 반응물 | Potassium alloy, nonbase, K,Na | HCID 16211683 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-(2-propynyl)-3-trifluoromethyl-1H-pyrrole-4-methanol | HCID 14370788 | 54.6% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04737513 |
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| 출처 데이터셋 | uspto-grants-1988_04 |
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| ORD ID | ord-bf7b0a646c1546ba9e56014f1a85bc9f |
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| 출처 메모 | uspto-grants-1988_04 |
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