関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | Indazole-3-carboxylic acid | HCID 78250 | — |
| 反応物 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-Methoxy-N-methyl-1H-indazole-3-carboxamide | HCID 16036867 | 81.4% |
反応手順
3-Carboxyindazole (10 g, 61.7 mmol) in DMF (100 mL) was treated with carbonyldiimidazole (11 g, 67.84 mmol) at rt with gas evolution for 15 min, after which the reaction mixture was heated up to 65° C. for 2 hours. After cooling to rt, N,O-dimethylhydroxyamine-HCl (4.14 g, 67.8 mmol) was added and the mixture was heated to 65° C. overnight. The reaction was cooled, quenched with water, extracted with CH2Cl2 and washed with water. The combined organic phase was dried and concentrated to afford N-methoxy-N-methyl-1H-indazole-3-carboxamide (10.3 g, 81.4%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08198456B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-c678d9ae3a624567bfad52efe9f10168 |
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| 出典メモ | uspto-grants-2012_06 |
|---|
