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Hydrochloric Acid → 4-methoxyacetoxy-1-phenyl-1,8-naphthyridin-2(1H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methoxyacetyl chloride | HCID 96623 | — |
| 反応物 | 4-Hydroxy-1-phenyl-1,8-naphthyridin-2(1H)-one | HCID 54686473 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-methoxyacetoxy-1-phenyl-1,8-naphthyridin-2(1H)-one | HCID 68948066 | 73% |
反応手順
In accordance with a process described in JP-61-246183A, 4-hydroxy-1-phenyl-1,8-naphthyridin-2(1H)-one was synthesized. To a suspension of the synthesized compound (893 mg, 3.7 mmol) in DMF (20 mL) was added sodium hydride (purity of about 60%, 192 mg, 4.8 mmol, 1.3 eq.), and the mixture was stirred until no more hydrogen was generated. Then, methoxyacetyl chloride (1.07 g, 9.9 mmol, 2.6 eq.) was added thereto, and the mixture was stirred at a room temperature for 50 minutes. To the mixture was added water. The resulting mixture was acidified with concentrated hydrochloric acid, and then the resulting precipitate was separated by filtration and dried to give 4-methoxyacetoxy-1-phenyl-1,8-naphthyridin-2(1H)-one (847 mg, yield 73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08193356B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-8cb787f441ec49de8defc03ca7d03e3b |
| 出典メモ | uspto-grants-2012_06 |