反应详情

After weighing 80 g (0.28 mol) of 1-benzyl-4-(4-fluorophenyl)-4-hydroxypiperidine and 69.0 g (0.364 mol) of p-toluenesulfonic acid monohydrate to 400 ml of chlorobenzene under stirring, the reaction mixture is boiled under reflux for 3 hours while distilling out water introduced as crystal water and the water formed in the reaction. After termination of the reaction, 100 ml of chlorobenzene are additionally distilled out under atmospheric pressure. After cooling the mixture obtained to 0° C., the precipitated title product is filtered, twice washed with 10 ml of cold acetone each and dried on the air to give a yield of 90.5 g (73%), m.p.: 180-182° C.

1. temperatureunder reflux for 3 hours
2. distillationwhile distilling out water
3. additionintroduced as crystal water
4. customthe water formed in the reaction
5. distillationare additionally distilled out under atmospheric pressure
6. temperatureAfter cooling the mixture
7. customobtained to 0° C.
8. customthe precipitated title product
9. filtrationis filtered
10. washtwice washed with 10 ml of cold acetone each and
11. customdried on the air
12. customto give a yield of 90.5 g (73%), m.p.: 180-182° C.