HRID1081262

反应详情

EQUATION

反应方程式

HRID 1081262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-fluoroaniline (5.0 g), potassium carbonate (2.5 g) and copper(I)iodide (414 mg) in 2-fluoronitrobenzene (16.9 ml) was heated to 180° under nitrogen for 18 h. The cooled mixture was poured into water (300 ml) and extracted with ethyl acetate (2×250 ml) then the combined extracts were washed with saturated brine and evaporated. The residual brown oil was azeotroped with ethanol/water then toluene. The residue was chromatographed with hexane-DE (100:0 to 95:5) to give the title compound (3.25 g) as a bright orange solid, m.p.58°-9°.

WORKUP

后处理

  1. temperaturewas heated to 180° under nitrogen for 18 h
  2. extractionextracted with ethyl acetate (2×250 ml)
  3. washthe combined extracts were washed with saturated brine
  4. customevaporated
  5. customThe residual brown oil was azeotroped with ethanol/water
  6. customThe residue was chromatographed with hexane-