참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzoyl Peroxide | HCID 7187 | — |
| 반응물 | N-bromobutanimide | HCID 67184 | — |
| 반응물 | Ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate | HCID 67390769 | — |
| 용매 | Carbon Tetrachloride | HCID 5943 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Ethyl 6-(bromomethyl)-2-(trifluoromethyl)pyrimidine-4-carboxylate | HCID 58431340 | — |
반응 단계
A mixture of ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate (1.1 g, 4.5 mmol, prepared as described in WO 2007/090748), N-bromosuccinimide (2.86 g, 16.1 mmol) and benzoyl peroxide (0.21 g, 0.9 mmol) in carbon tetrachloride (9 mL) was heated in a sealed vessel to 100° C. overnight. The mixture was diluted with dichloromethane (DCM), filtered and the solvent was removed in vacuo. Purification via preparative HPLC-MS (C18 eluting with a gradient of MeCN/H2O containing 0.15% NH4OH) afforded the product, which on removal of solvent, was an oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08765734B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_07 |
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| ORD ID | ord-f728d6ece63f461a8adbc30112a9ffb4 |
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| 출처 메모 | uspto-grants-2014_07 |
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