反应详情

温度

250 °C

4-(2,3-Dichlorobenzyl)phenylamine (10.0 g, 39.7 mmol) obtained in Step 2 was dissolved in toluene (100 ml) and diethyl ethoxymethylenemalonate (8.8 ml, 43.7 mmol) was added. The mixture was heated under reflux for 3 hrs. The reaction solution was concentrated under reduced pressure, and diphenyl ether (100 ml) was added to dissolve the residue. The mixture was stirred with heating at 250° C. for 3 hrs. After allowing the mixture to cool, n-hexane was added to the reaction solution and the precipitate was collected by filtration, washed with chloroform and vacuum-dried to give an object product (10.1 g, yield 68%) as a pale-yellow solid.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 3 hrs
3. concentrationThe reaction solution was concentrated under reduced pressure, and diphenyl ether (100 ml)
4. additionwas added
5. dissolutionto dissolve the residue
6. temperatureto cool
7. additionn-hexane was added to the reaction solution
8. filtrationthe precipitate was collected by filtration
9. washwashed with chloroform
10. customvacuum-dried