反应详情

温度

80 °C

The crude ethyl 4-(2-(4-tolylsulfanyl)phenyl)-piperidin-1-carboxylate as a red oil from example 3 was mixed in a stirred reactor with hydrobromic acid in acetic acid (40%, 545 mL, 3.11 mol). The mixture was heated at 80° C. for 18 hours. The reaction mixture was cooled down to room temperature. During the cooling the product crystallises out. After 1 hour at room temperature ethyl ether (800 mL) was added to the reaction mixture, and the mixture was stirred for another hour. The product was filtered off, washed with ethyl ether and dried in a vacuum oven at 50° C. until constant weight.

1. temperatureThe reaction mixture was cooled down to room temperature
2. customDuring the cooling the product crystallises out
3. additionAfter 1 hour at room temperature ethyl ether (800 mL) was added to the reaction mixture
4. filtrationThe product was filtered off
5. washwashed with ethyl ether
6. customdried in a vacuum oven at 50° C. until constant weight