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Methyl iodide → 4-[4-(Methylsulfonyl)phenyl]-N-methyl-N-tetrahydro-2H-pyran-4-yl-6-(trifluoromethyl)pyrimidin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-(4-(methylsulfonyl)phenyl)-N-(tetrahydro-2H-pyran-4-yl)-6-(trifluoromethyl)pyrimidin-2-amine | HCID 9822357 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[4-(Methylsulfonyl)phenyl]-N-methyl-N-tetrahydro-2H-pyran-4-yl-6-(trifluoromethyl)pyrimidin-2-amine | HCID 10136579 | — |
反応手順
A solution of 4-[4-(methylsulfonyl)phenyl]-N-tetrahydro-2H-pyran-4-yl-6-(trifluoromethyl)pyrimidin-2-amine (0.05 g) in dry dimethylformamide (2 ml) was treated with sodium hydride (0.007 g, 60% in mineral oil) and the mixture stirred at ambient temperature for 30 minutes. Iodomethane (0.01 ml) was added and the mixture stirred overnight. The reaction mixture was concentrated in vacuo and the residue partitioned between dichloromethane (20 ml) and water (20 ml). The organic layer was purified by passing through a silica bond elute column and eluting with dichloromethane. Concentration of the eluent gave the title compound as a yellow solid (0.031 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084148B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-7489cadc00124f82a4089f651da7299f |
| 出典メモ | uspto-grants-2006_08 |