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Benzyl Alcohol → 2-(Benzyloxy)-N-(2,4-dimethoxybenzyl)pyrimidin-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | N-(2,4-dimethoxybenzyl)-2-fluoropyrimidin-4-amine | HCID 89963279 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(Benzyloxy)-N-(2,4-dimethoxybenzyl)pyrimidin-4-amine | HCID 89962868 | 99% |
反応手順
To a solution of the N-(2,4-dimethoxybenzyl)-2-fluoropyrimidin-4-amine (2.50 g, 9.50 mmol) prepared in Example 95a and benzyl alcohol (1.97 mL, 19.0 mmol) in DMF (48 mL), sodium hydride (0.90 g, 23.7 mmol) was added, and the reaction solution was stirred at room temperature for 6 hours. To the reaction solution, an aqueous ammonium chloride solution (200 mL) was added, followed by extraction with ethyl acetate (100 mL). The thus obtained organic layer was washed twice with water (200 mL) and dried over anhydrous sodium sulfate. After vacuum concentration, the residue was purified with silica gel chromatography (hexane/ethyl acetate=1:2) to yield the title compound (3.29 g, 99%) as a colorless amorphous solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889741B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-7b3ea41c23bc417593694accaf015a27 |
| 出典メモ | uspto-grants-2014_11 |