反应详情

温度

0 °C

To a suspension of 3-chloro-2,4-dimethyl-aniline (0.47 g, 3.0 mmol), in a mixture of water (3 mL) and conc. H2SO4 (2 ml), a solution of Na2NO2 (0.22 g) in H2O (5 ml) was added dropwise at 0° C. The mixture was stirred 1 h at 0° C., than treated with urea (0.2 g), stirred for 10 min at 0° C. A solution of CuSO4 (1.0 g) in water (6 mL) was added and the mixture was stirred for 60 h at RT. The reaction mixture was extracted with CH2Cl2 (2×20 ml), extracts were dried over Na2SO4 and evaporated. The residue was separated on SiO2 (4.0 g) column, hexane-EtOAc (0 to 10%). Brown crystals, 45 mg (0.29 mmol, 10%).

1. stirringstirred for 10 min at 0° C
2. stirringthe mixture was stirred for 60 h at RT
3. extractionThe reaction mixture was extracted with CH2Cl2 (2×20 ml), extracts
4. dry with materialwere dried over Na2SO4
5. customevaporated
6. customThe residue was separated on SiO2 (4.0 g) column, hexane-EtOAc (0 to 10%)