HRID734703

反应详情

EQUATION

反应方程式

HRID 734703 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Fluoro-5-nitroindazole (850 mg, 4.693 mmol, 1.0 equiv) was dissolved in 20 mL EtOH, NaOCl (10 mL, 164.26 mmol, 35 equiv) was added and the reaction mixture was stirred at room temperature for 3 hours. The reaction mixture was concentrated en vacuo to remove EtOH was then diluted with EtOAc and water. The phases were separated, and the organic phase was washed once with satd. NaHCO3, and once with satd. NaCl. The organic phase was dried over Na2SO4, filtered, and concentrated en vacuo. The residue was purified by flash chromatography (10-100% EtOAc in Hexanes) to provide 583 mg (58%) of the title compound as a light orange solid. MS (ES+) m/e 216 [M+H]+

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated en vacuo
  2. customto remove EtOH
  3. additionwas then diluted with EtOAc and water
  4. customThe phases were separated
  5. washthe organic phase was washed once with satd
  6. dry with materialThe organic phase was dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated en vacuo
  9. customThe residue was purified by flash chromatography (10-100% EtOAc in Hexanes)