참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | Ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate | HCID 67390769 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | Ethyl 6-(bromomethyl)-2-(trifluoromethyl)pyrimidine-4-carboxylate | HCID 58431340 | — |
반응 단계
A solution of ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate (2.00 g, 8.54 mmol, prepared as described in WO2007/090748) in acetic acid (12 mL) was treated with bromine (1.36 g, 8.54 mmol) and the reaction was heated to 80° C. in a sealed vial for 30 minutes, at which time, the color of bromine was dissipated. The acetic acid was removed in vacuo and was followed by dissolving of the residue in toluene and removal of solvent in vacuo. The percent by weight of desired component in the mixture (containing unreacted starting material and overbrominated product) was determined by NMR and the mixture used without further purification (1.62 g, 61%). 1H NMR (300 MHz, CDCl3): δ 8.32 (s, 1H), 4.60 (s, 2H), 4.54 (q, 2H), 1.46 (t, 3H); LCMS (M+H)+: 313.0, 315.0
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08933085B2 |
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| 출처 데이터셋 | uspto-grants-2015_01 |
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| ORD ID | ord-0a72c58090a64fdbb1ebd67d96e5bb41 |
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| 출처 메모 | uspto-grants-2015_01 |
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