反应详情

温度

75 °C

A mixture of 4-(4-methoxy-2-nitrophenylazo)benzene-1,3-diol (2.5 g, i.e. 0.0086 mol) and potassium carbonate (1.24 g) in 30 ml of dimethylformamide was brought to 70-75° C. 3-Chloropropyltrimethylsilane (1.24 g, i.e. 0.0086 mol) was added thereto over 20 minutes. The mixture was stirred at 75° C. for 6 hours. The reaction mixture was then poured into 50 ml of water and extracted with diisopropyl ether. The organic phase was dried, concentrated and purified by column chromatography (eluent: 50/50 heptane/CH2Cl2) to give compound (9) in the form of a red powder.

1. customwas brought to 70-75° C
2. extractionextracted with diisopropyl ether
3. customThe organic phase was dried
4. concentrationconcentrated
5. custompurified by column chromatography (eluent: 50/50 heptane/CH2Cl2)