HRID924563

反应详情

EQUATION

反应方程式

HRID 924563 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

9-Fluoro-6-Phenanthridinamine (0.8 g, 3.7 mmol), and a 50% solution of acetyl chloride (0.4 g, 5.66 mmol) in water containing sodium bicarbonate (0.6 g, 7.54 mmol) was dissolved in isopropyl alcohol (25 mL). The reaction mixture was refluxed for 17 hours under a nitrogen pad. The reaction mixture was cooled to room temperature and the precipitate vacuum filtered and washed with methylene chloride. The crude product was purified by column chromatography using a 1:1 ratio of ethyl acetate and hexanes as the eluants followed by distillation to give 10-fluoro-imidazo[1,2-f]phenanthridine) (0.46 g, 52% yield).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 17 hours under a nitrogen pad
  2. filtrationthe precipitate vacuum filtered
  3. washwashed with methylene chloride
  4. customThe crude product was purified by column chromatography
  5. distillationfollowed by distillation