反应详情

温度

65 °C

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%).

1. temperatureAfter cooling to rt
2. temperaturethe mixture was heated to 65° C. overnight
3. temperatureThe reaction was cooled
4. customquenched with water
5. extractionextracted with CH2Cl2
6. washwashed with water
7. customThe combined organic phase was dried
8. concentrationconcentrated