反应详情

Tris-(dibenzylidene-acetone)-dipalladium (0.03 mmol), (2′-dicyclohexylphosphanyl-biphenyl-2-yl)-dimethyl-amine (0.9 mmol) and NaOtBu (6.5 mmol) are suspended in toluene (20 ml) in an oxygen-free atmosphere (N2). 4-Bromo-benzoic acid methyl ester (4.65 mmol) and 1-(benzyl)-piperazine (5.6 mmol) are added and the stirred mixture is heated under reflux for 4 hours. After cooling, a mixture of ethylacetate and diethylether is added and the mixture is filtered. Then the solvent is evaporated and the residue is suspended in diethylether and the solid filtered of and dried (vacuum). A pale powder with mp. 105-107° C., Rf=0.67 (CH2Cl2/MeOH=95:5) is obtained.

1. temperaturethe stirred mixture is heated
2. temperatureunder reflux for 4 hours
3. temperatureAfter cooling
4. additionis added
5. filtrationthe mixture is filtered
6. customThen the solvent is evaporated
7. filtrationthe solid filtered of and
8. customdried (vacuum)
9. customA pale powder with mp. 105-107° C., Rf=0.67 (CH2Cl2/MeOH=95:5) is obtained