反应详情

1-Benzyl-4-(4-trifluoromethylphenyl)-1,2,3,6-tetrahydropyridine (2 g, 6.3 mmol) prepared in Reference Example 96 was dissolved in methylene chloride (20 ml), to which 2-chloroethyl chloroformate (1.67 g, 11.68 mmol) was added dropwise under a nitrogen atmosphere while cooling in an ice-bath, and the mixture was stirred at the same temperature for 3 hours. Methanol (20 ml) was added to the mixture, which was heated under reflux for 1 hour. The reaction mixture was allowed to return to room temperature, to which diethyl ether was added, and the resulting precipitates were collected by filtration to afford 4-(4-trifluoromethylphenyl)-1,2,3,6-tetrahydropyridine hydrochloride (1.44 g, yield 87%) as a colorless crystalline powder.

1. additionwas added dropwise under a nitrogen atmosphere
2. temperaturewhile cooling in an ice-bath
3. temperaturewas heated
4. temperatureunder reflux for 1 hour
5. additionwas added
6. customthe resulting precipitates
7. filtrationwere collected by filtration