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Thiomorpholine → 1,1,1-Trifluoro-4(5-fluoro-2-methoxyphenyl)-4-methyl-2-thiomorpholin-4-ylmethylpentan-2-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiomorpholine | HCID 67164 | — |
| 反応物 | 2-[2-(5-Fluoro-2-methoxyphenyl)-2-methylpropyl]-2-trifluoromethyloxirane | HCID 16099239 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,1,1-Trifluoro-4(5-fluoro-2-methoxyphenyl)-4-methyl-2-thiomorpholin-4-ylmethylpentan-2-ol | HCID 10453296 | — |
反応手順
A solution of 2-[2-(5-fluoro-2-methoxyphenyl)-2-methylpropyl]-2-trifluoromethyloxirane (see Example 1) (130 mg) and thiomorpholine (84.6 μL) in dimethylformamide (1 μL) was heated at 100° C. for 15 hours. The resulting mixture was diluted with diethyl ether, washed with water and brine, dried over sodium sulfate, filtered, and the volatiles removed in vacuo. The residue was purified by silica gel column chromatography using 2% EtOAc-hexanes as the eluent. The product-rich fractions were concentrated in vacuo to provide the title compound as a clear oil (161 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07579469B2 |
| 出典データセット | uspto-grants-2009_08 |
| ORD ID | ord-2553ffd9f11c47ecb6e10b1c9e799b20 |
| 出典メモ | uspto-grants-2009_08 |