참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4,6-Dichloro-2-(methylthio)pyrimidine | HCID 80531 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-Ethoxy-2-methylthio-6-[3-(trifluoromethyl)phenoxy]pyrimidine | HCID 19693868 | — |
반응 단계
Ethanol (1.18 g, 0.0256×1.0 mol) and NaH (1.02 g, (ca.60% in mineral oil), 0.0256×1.0 mol) were dissolved in THF and 4,6-dichloro-2-methylthiopyrimidine (Compound No. VII-23)(5.0 g, 0.0256 mol) was added thereto. The resulting solution was stirred for about 30 minutes at room temperature. To this reaction solution, m-trifluoromethyl-phenol (6.23 g, 0.0256×1.5 mol), NaH (1.54 g, (ca.60% in mineral oil), 0.0256×1.5 mol), and KI (2.12 g, 0.0256×0.5 mol) dissolved in DMF were added. The resulting solution was refluxed for about 7 hours. The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate to separate an organic phase. The organic phase was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, and thereafter purified on a silica gel column.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05723412 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-0c41a886f892437a80e1ebfc69bc8999 |
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| 출처 메모 | uspto-grants-1998_03 |
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