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Sodium Carbonate → 3-(2,6-dichloro-3-nitro-phenyl)-1H-[1,6]naphthyridin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-(2,6-dichloro-3-nitro-phenyl)-N-(3-formyl-pyridin-4-yl)-acetamide | HCID 59833859 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-(2,6-dichloro-3-nitro-phenyl)-1H-[1,6]naphthyridin-2-one | HCID 59833918 | 79% |
反応手順
A solution of 2-(2,6-dichloro-3-nitro-phenyl)-N-(3-formyl-pyridin-4-yl)-acetamide (5.0 g, 14.12 mmol) and Na2CO3 (2.5 g) in MeOH (300 mL) is heated for 15 minutes at 70° C. After filtration of the reaction mixture, the solvent is removed by concentration to give crude product, which is purified by flash silica gel column elute with CH2Cl2 (100%) gradient to CH2Cl2/MeOH (2N NH3) (93/7%) to give the titled intermediate as a solid (3.75 g, 77.7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07449582B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-4b99fbcd4e8446b9be2e524b54b79be4 |
| 出典メモ | uspto-grants-2008_11 |