関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate | HCID 67390769 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 6-(bromomethyl)-2-(trifluoromethyl)pyrimidine-4-carboxylate | HCID 58431340 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08765734B2 |
|---|
| 出典データセット | uspto-grants-2014_07 |
|---|
| ORD ID | ord-f728d6ece63f461a8adbc30112a9ffb4 |
|---|
| 出典メモ | uspto-grants-2014_07 |
|---|
