反应详情

温度

100 °C

Dissolve 1-bromo-4-methyl-2-pentanone (11.0 g, 61.4 mmol) and potassium phthalimide (11.9 g, 64.5 mmol) in toluene (60 mL) at room temperature under a nitrogen atmosphere. Heat the mixture to 100° C. and stir for 16 h. Cool the resulting slurry to room temperature, filter off solids, and concentrate the filtrate in vacuo to a solid. Purify the residue by chromatography on silica gel (40 g) eluting with hexane/EtOAc (1:1) to obtain the desired intermediate (3.6 g, 24%). MS (ES+) m/z: 246.3 (M+H)+.

1. temperatureCool the resulting slurry to room temperature
2. filtrationfilter off solids
3. concentrationconcentrate the filtrate in vacuo to a solid
4. customPurify the residue by chromatography on silica gel (40 g)
5. washeluting with hexane/EtOAc (1:1)