反应详情

温度

100 °C

A mixture of 3-chloro-4-anisidine (Aldrich; 0.633 g), bis(2-chloroethyl)amine hydrochloride (Aldrich; 0.860 g), potassium carbonate (1.11 g), and N,N-dimethylacetamide (6 mL) is stirred at 100° C. for 17.5 h, at which time the mixture is cooled and partioned between dichloromethane and water/sodium bicarbonate. The organic layers are dried over sodium sulfate, concentrated, and the residue is chromatographed on silica gel using methanol/dichloromethane (8/92) to give 0.297 g of 1-(3-chloro-4-methoxyphenyl)piperazine. 1H NMR (CDCl3) δ3.05, 3.86, 6.80, 6.87, 6.99.

1. temperatureis cooled
2. dry with materialThe organic layers are dried over sodium sulfate
3. concentrationconcentrated
4. customthe residue is chromatographed on silica gel