HRID1790157

反应详情

EQUATION

反应方程式

HRID 1790157 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturewas heated until a red solution
  2. customformed
  3. additionwas added
  4. extractionextracted with ethyl acetate
  5. washThe combined organic layer was washed with H2O
  6. concentrationconcentrated under reduced pressure
  7. custompurified by flash chromatography