反应详情

A mixture of 1-formyl-4-(2-bromo-4-methoxyphenyl)piperazine (VII, 3.92 g, 3.1 mmol) and hydrochloric acid (4N, 70 ml) is heated at 100° for 50 min. The mixture is then concentrated under reduced pressure to remove most of the aqueous hydrochloric acid. Saturated sodium bicarbonate is then cautiously added and the aqueous phase is extracted with dichloromethane. The combined organic phase is backwashed with saline, dried over magnesium sulfate, and concentrated to give 1-(2-bromo-4-methoxyphenyl)piperazine (VIII), NMR (CDCl3) 2.55, 2.95, 3.08, 3.77, 6.83, 7.01, 7.14 δ.

1. temperatureis heated at 100° for 50 min
2. concentrationThe mixture is then concentrated under reduced pressure
3. customto remove most of the aqueous hydrochloric acid
4. additionSaturated sodium bicarbonate is then cautiously added
5. extractionthe aqueous phase is extracted with dichloromethane
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated