反应详情

温度

70 °C

7-ethoxy-N-(3-ethynylphenyl)-6-nitroquinazolin-4-amine (8 g, 0.024 mol) was dissolved in a mixture of 80 ml ethanol, 80 ml H2O and 10 ml acetic acid. The reaction was heated to 70° C., then Fe (5.4 g, 0.096 mol) was added. The reaction mixture was heated to reflux for 4 hours. The resulting clear reaction solution was concentrated under reduced pressure to remove solvent. The pH of the residue was adjusted to 9 with 4N aqueous NaOH, and was washed with 200 ml EA/MeOH (50/1) until TLC show no product can be detected in the organic layer. The combined organic layers were concentrated, grey solid was precipitated and filtered to afford 7-ethoxy-N4-(3-ethynylphenyl)quinazoline-4,6-diamine as grey solid 5.4 g (74.2% yield).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 4 hours
3. concentrationThe resulting clear reaction solution was concentrated under reduced pressure
4. customto remove solvent
5. washwas washed with 200 ml EA/MeOH (50/1) until TLC
6. concentrationThe combined organic layers were concentrated
7. customgrey solid was precipitated
8. filtrationfiltered