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Sodium Carbonate → 2-(4-nitro-phenyl)-7-methoxy-1H-benzoimidazole-4-carboxylic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 反応物 | HCID 178498286 | HCID 178498286 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(4-nitro-phenyl)-7-methoxy-1H-benzoimidazole-4-carboxylic acid methyl ester | HCID 58624190 | 46.1% |
反応手順
3-[(4-nitro-benzimidoyl)-amino]-4-methoxy-benzoic acid methyl ester (1.63 g, 4.95 mmol) was dissolved in 50% methanol, and 5% NaOCl was added dropwise thereto at room temperature. After checking the reaction by TLC, Na2CO3 (1.05 g, 9.38 mmol) seas added dropwise thereto and refluxed for 40 min. The resulting solution was cooled to room temperature, extracted with ethyl acetate and the extract was concentrated under a reduced pressure. The resulting residue was purified by silica gel column chromatography to obtain the title compound (0.75 g, 2.28 mmol) in a yield of 46%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179832B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-f504fecf8c0247e4ae3d761ac9265e77 |
| 出典メモ | uspto-grants-2007_02 |