反应详情

温度

100 °C

Reaction of propiophenone with p-tolyltosylate: Pd(OAc)2 (9.0 mg, 0.040 mmol), ligand (27.1 mg, 0.050 mmol), NaOtBu (144 mg, 1.50 mmol) and 4-methylphenyl-p-toluene sulfonate (262 mg, 1.00 mmol) were suspended in 1 mL of dioxane in a screw-capped vial. The vial was sealed with a cap containing a PTFE septum and removed from the dry box. Propiophenone (132 mg, 1.10 mmol) was added to the reaction mixture by syringe. The reaction mixture was stirred at 100° C. and monitored by GC analysis. The crude reaction was diluted with ether and washed with 1N HCl, water and brine. The organic layer was dried over Na2SO4, filtered and concentrated in vacuo. The residue was chromatographed on silica gel (hexane/EtOAc=95/5) to give 135 mg (60%) of 2-(4-Methoxyphenyl)-1-phenyl-1-propanone.

1. customThe vial was sealed with a cap
2. customremoved from the dry box
3. customThe crude reaction
4. washwashed with 1N HCl, water and brine
5. dry with materialThe organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue was chromatographed on silica gel (hexane/EtOAc=95/5)