3-溴-1-(2,2,2-三氟乙基)吡咯烷-2-one

反应条件: temp:5.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 189 g (0.77 Mol) rac-3-Bromo-1-(2,2,2-trifluoroethyl)-2-pyrrolidone were dissolved in 1 l toluene, and 222 g (0.85 Mol) triphenylphosphine were added. The mixture was refluxed over-night in an argon atmosphere, the product starting to precipitate. The mixture was then cooled to 5° C. and the slightly brownish crystals were filtered off. They were stirred twice in 1 l THF, filtered and dried in a vacuum at 50° C. Yield: 308 g (79%) colorless crystals 1H-NMR (3): δ[ppm]2.17 (m, 1 H); 3.2-3.5 (m, 3 H); 3.93 (dd, 1H); 4.24 m, 1H); 6.91 (m, 1H); 7.60-8.03 (arom., m, 15H). IR (KBr): 1690 cm-1 MS(ISP): 428.3 (M+) The mixture was refluxed over-night in an argon atmosphere to precipitate the slightly brownish crystals were filtered off filtered dried in a vacuum at 50° C

反应条件: temp:5.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 189 g (0.77 Mol) rac-3-Bromo-1-(2,2,2-trifluoroethyl)-2-pyrrolidone were dissolved in 1 l toluene, and 222 g (0.85 Mol) triphenylphosphine were added. The mixture was refluxed over-night in an argon atmosphere, the product starting to precipitate. The mixture was then cooled to 5° C. and the slightly brownish crystals were filtered off. They were stirred twice in 1 l THF, filtered and dried in a vacuum at 50° C. Yield: 308 g (79%) colorless crystals 1H-NMR (3): δ[ppm]2.17 (m, 1 H); 3.2-3.5 (m, 3 H); 3.93 (dd, 1H); 4.24 m, 1H); 6.91 (m, 1H); 7.60-8.03 (arom., m, 15H). IR (KBr): 1690 cm-1 MS(ISP): 428.3 (M+) The mixture was refluxed over-night in an argon atmosphere to precipitate the slightly brownish crystals were filtered off filtered dried in a vacuum at 50° C

反应条件: temp:5.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 189 g (0.77 Mol) rac-3-Bromo-1-(2,2,2-trifluoroethyl)-2-pyrrolidone were dissolved in 1 l toluene, and 222 g (0.85 Mol) triphenylphosphine were added. The mixture was refluxed over-night in an argon atmosphere, the product starting to precipitate. The mixture was then cooled to 5° C. and the slightly brownish crystals were filtered off. They were stirred twice in 1 l THF, filtered and dried in a vacuum at 50° C. Yield: 308 g (79%) colorless crystals 1H-NMR (3): δ[ppm]2.17 (m, 1 H); 3.2-3.5 (m, 3 H); 3.93 (dd, 1H); 4.24 m, 1H); 6.91 (m, 1H); 7.60-8.03 (arom., m, 15H). IR (KBr): 1690 cm-1 MS(ISP): 428.3 (M+) The mixture was refluxed over-night in an argon atmosphere to precipitate the slightly brownish crystals were filtered off filtered dried in a vacuum at 50° C

反应条件: temp:5.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 189 g (0.77 Mol) rac-3-Bromo-1-(2,2,2-trifluoroethyl)-2-pyrrolidone were dissolved in 1 l toluene, and 222 g (0.85 Mol) triphenylphosphine were added. The mixture was refluxed over-night in an argon atmosphere, the product starting to precipitate. The mixture was then cooled to 5° C. and the slightly brownish crystals were filtered off. They were stirred twice in 1 l THF, filtered and dried in a vacuum at 50° C. Yield: 308 g (79%) colorless crystals 1H-NMR (3): δ[ppm]2.17 (m, 1 H); 3.2-3.5 (m, 3 H); 3.93 (dd, 1H); 4.24 m, 1H); 6.91 (m, 1H); 7.60-8.03 (arom., m, 15H). IR (KBr): 1690 cm-1 MS(ISP): 428.3 (M+) The mixture was refluxed over-night in an argon atmosphere to precipitate the slightly brownish crystals were filtered off filtered dried in a vacuum at 50° C