HRID1747796

反应详情

EQUATION

反应方程式

HRID 1747796 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 6-[3-(trifluoromethyl)phenyl]pyridazin-3(2H)-one (240 mg), 5-iodo-1-phenyl-1H-pyrazole (540 mg), copper powder (64 mg) and potassium carbonate (415 mg) in pyridine (5 mL) was heated under reflux for 24 hr. The reaction mixture was poured into 1M hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) and recrystallized from hexane/ethyl acetate to give the title compound (56.5 mg).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 24 hr
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)
  8. customrecrystallized from hexane/ethyl acetate