反应详情

温度

100 °C

(2-Chloro-4-mercapto-phenoxy)-acetic acid ethyl ester (3 g; 12.16 mmol), dibromo-phenol (3.67 g; 14.59 mmol), tris(dibenzylideneacetone)dipalladium (0) (0.45 g; 0.49 mmol), and 1,1′-bis-(diphenylphosphino)ferrocene (0.40 g; 0.73 mmol) were added to a dry reaction flask under an atmosphere of nitrogen. Triethylamine (6.74 mL, 48.64 mmol) and NMP (10 mL) were added, and the reaction mixture was stirred in a microwave oven for 1 h at 100° C. The reaction mixture was extracted with ethyl acetate, and the ethyl acetate phase was washed twice with a 5% aqueous citric acid solution. The organic phase was dried and evaporated in vacuo. The crude reaction product was purified by flash chromatography (dichloromethane→dichlormethane:ethyl acetate (1:1)). Yield 1.8 g. HPLC-MS: m/z: 441.2 (M+Na); Rt: 2.34 min.

1. extractionThe reaction mixture was extracted with ethyl acetate
2. washthe ethyl acetate phase was washed twice with a 5% aqueous citric acid solution
3. customThe organic phase was dried
4. customevaporated in vacuo
5. customThe crude reaction product
6. customwas purified by flash chromatography (dichloromethane→dichlormethane:ethyl acetate (1:1))