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) δ 3.05, 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