HRID1081262
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated to 180° under nitrogen for 18 h
- extractionextracted with ethyl acetate (2×250 ml)
- washthe combined extracts were washed with saturated brine
- customevaporated
- customThe residual brown oil was azeotroped with ethanol/water
- customThe residue was chromatographed with hexane-