関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Hydratropoyl chloride | HCID 2760403 | — |
| 反応物 | 4-hydroxy-1-(3-trifluoromethoxyphenyl)-1,8-naphthyridin-2(1H)-one | HCID 68947271 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 68951216 | HCID 68951216 | — |
反応手順
In accordance with a process described in JP-61-246183A, 4-hydroxy-1-(3-trifluoromethoxyphenyl)-1,8-naphthyridin-2(1H)-one was synthesized. To a suspension of the synthesized compound (967 mg, 3.0 mmol) in DMF (24 mL) was added sodium hydride (purity of about 60%, 120 mg, 1.0 eq.). The mixture was stirred until no more hydrogen was generated, to obtain a solution. Then, 2-phenylpropionyl chloride (1.2 eq.) was added thereto, and the mixture was stirred at a room temperature for 1 hour. To the mixture was added a saturated sodium hydrogencarbonate aqueous solution, and the resulting precipitate was separated by filtration, washed with water, and dried to give 4-(2-phenylpropionyloxy)-1-(3-trifluoromethoxyphenyl)-1,8-naphthyridin-2(1H)-one as a form of crystal (1.14 g, yield 84%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08193356B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-7184c74a6fd446eebef6ee7c63ab62c3 |
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| 出典メモ | uspto-grants-2012_06 |
|---|