反应详情

温度

50 °C

Combine isopropanol (500 g), 2,2,3,3-tetrafluoropropylbenzaldehyde (116.8 g), and 6-fluorotryptamine (1.15 equiv.). Heat to reflux over about 1.5 hour. After 30 minutes at the reflux, distill and over 30 minutes collect about 380 g of distillate. Cool the reaction mixture to 50° C. and add NaBH4 (19.71 g) in one portion. After 1 hour at 50° C., slowly add water over 15 minutes and allow the resulting solution to cool to room temperature overnight. Distill the isopropanol under reduced pressure to give a residue and extract with dichloromethane, combine organic layers, and treat with 1N aqueous HCl (650 mL) to give a solid. Stir the heavy suspension for 2 hours at 20–25° C. Collect the solid by filtration, wash with dichloromethane and dry at 50° C. under vacuum overnight to afford title compound.

1. temperatureHeat
2. temperatureto reflux over about 1.5 hour
3. distillationdistill and over 30 minutes
4. distillationcollect about 380 g of distillate
5. additionadd NaBH4 (19.71 g) in one portion
6. waitAfter 1 hour at 50° C.
7. waitslowly add water over 15 minutes
8. temperatureto cool to room temperature overnight
9. distillationDistill the isopropanol under reduced pressure
10. customto give a residue
11. extractionextract with dichloromethane
12. additiontreat with 1N aqueous HCl (650 mL)
13. customto give a solid
14. customCollect the solid
15. filtrationby filtration
16. washwash with dichloromethane
17. customdry at 50° C. under vacuum overnight