反应详情

温度

0 °C

A solution of 2-chloroquinazoline (5 g) in 20 mL of toluene is added dropwise to a refluxing solution of piperazine (20 g) in 150 mL of toluene. The solution is heated for an additional 24 hours. After cooling to 0° C. for about 30 minutes, the solution is filtered. The filtrate is extracted with 10% acetic acid. The aqueous extracts are washed with ether, basified and extracted with toluene. The toluene layer is then washed with water, dried and concentrated. The resulting material is placed under vacuum overnight to afford the title compound (6.8 g, m.p. 64-66° C.). 1H NMR (CDCl3) 9.0 (s, 1H) , 7.66 (m, 2H), 7.56 (d, J=8 Hz, 1H), 7.22 (ddd, J=8,7,1 Hz, 1H), 4.0 (t, J=5 Hz, 4H), 3.05 (t, J=5 Hz, 4H).

1. temperatureThe solution is heated for an additional 24 hours
2. filtrationthe solution is filtered
3. extractionThe filtrate is extracted with 10% acetic acid
4. washThe aqueous extracts are washed with ether
5. extractionextracted with toluene
6. washThe toluene layer is then washed with water
7. customdried
8. concentrationconcentrated
9. customis placed under vacuum overnight