反应详情

Gaseous hydrochloric acid is introduced for 10 min into a round bottom flask containing 11.2 g (22.6 mmol) of 3-[4-(3-chlorophenyl]piperazin-1-yl]-N-(triphenylmethyl)propanamine and 300 ml of methanol, while the mixture is cooled in a bath of iced water. The mixture is allowed to return to room temperature and is then heated under reflux for 5.5 h. The solution is reduced to half its volume and is allowed to cool. The solid which precipitates is filtered off, is treated with water and aqueous ammonia, the mixture is extracted with ethyl acetate, the organic phase is washed with water and is dried and the solvent is evaporated off. 3.9 g of light yellow oil are obtained.

1. customto return to room temperature
2. temperatureis then heated
3. temperatureunder reflux for 5.5 h
4. temperatureto cool
5. customThe solid which precipitates
6. filtrationis filtered off
7. additionis treated with water and aqueous ammonia
8. extractionthe mixture is extracted with ethyl acetate
9. washthe organic phase is washed with water
10. customis dried
11. customthe solvent is evaporated off