反应详情

温度

97.5 °C

3,4-dimethoxybenzyl chloride (10 g, 53.6 mmol) was combined with piperazine (2.3 g, 26.8 mmol) in anhydrous DMF (30 ml) and heated with stirring under nitrogen for 8 hours at 95-100° C. The cooled reaction mixture was diluted with water (100 ml) and acidified to pH 1 with concentrated hydrochloric acid. The white precipitate was collected by filtration and washed with water (50 ml). The solid was re-suspended in water (50 ml) and the pH adjusted to >9 by the dropwise addition of sodium hydroxide solution (50% NaOH in water). The resultant white solid was collected by filtration and dried under vacuum at 50° C., yield 10 g.

1. temperatureheated
2. customThe cooled reaction mixture
3. filtrationThe white precipitate was collected by filtration
4. washwashed with water (50 ml)
5. additionthe pH adjusted to >9 by the dropwise addition of sodium hydroxide solution (50% NaOH in water)
6. filtrationThe resultant white solid was collected by filtration
7. customdried under vacuum at 50° C.