反应详情

Triethylamine (1.5 ml) was added to a solution of (+)-1-benzyl-3-hydroxymethyl-4-(4-fluorophenyl)-1,2,3,6-tetrahydropyridine (2.82 g) in toluene (22.18 g) and the mixture was stirred at ambient temperature. The solution was cooled to 5° C. in an ice/water bath and the trifluoromethanesulphonic anhydride (1.8 ml) was added dropwise over 5 minutes. The mixture was stirred at 0° C. to room temperature for 4 hours, then stood for 48 hours. Water (25 ml) was added. The mixture was stirred for 2 minutes and then ethyl acetate and 4M-NaOH were added to dissolve an insoluble oil. The organic layer was separated, washed with water (25 ml), and then dried, filtered and evaporated to give 1-benzyl-4-(4-fluorophenyl)-1-azoniabicyclo[3.1.1]hept-3-ene trifluoro-methanesulphonate as an oil The oil was triturated with 60-80° C. petrol to give a solid.

1. temperatureThe solution was cooled to 5° C. in an ice/water bath
2. stirringThe mixture was stirred at 0° C. to room temperature for 4 hours
3. stirringThe mixture was stirred for 2 minutes
4. dissolutionto dissolve an insoluble oil
5. customThe organic layer was separated
6. washwashed with water (25 ml)
7. customdried
8. filtrationfiltered
9. customevaporated