HRID1790157
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a mixture of NaOH (0.500 g, 12.5 mmol) in H2O (15.0 mL) was added 4-nitroindazole (0.500 g, 3.07 mmol) after which it was heated until a red solution formed. The solution was immediately placed in an ice-water bath for 15 minutes before NaClO (6.00 mL, 5.25%, 4.50 mmol) was added. The mixture was stirred at 0° C. for 5 hour, the pH adjusted to 7 with dilute HCl and extracted with ethyl acetate. The combined organic layer was washed with H2O, concentrated under reduced pressure and purified by flash chromatography to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 8.17 (m, 1H), 8.57 (m, 1H), 8.77 (m, 1H), 14.17 (s, 1H); MS (DCI/NH3) m/Z 197[M+H]+.
WORKUP
后处理
- temperaturewas heated until a red solution
- customformed
- additionwas added
- extractionextracted with ethyl acetate
- washThe combined organic layer was washed with H2O
- concentrationconcentrated under reduced pressure
- custompurified by flash chromatography