2,2-色满-7-氯色满-4-酮

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

实验步骤: A solution of 4-chloro-2-hydroxyacetophenone (20 g, 0.1176 mol), acetone (13.3 mL, 0.1811 mol) and pyrrolidine (15 mL, 0.18 mol) in methanol (475 mL) was stirred at 25° C. overnight. The mixture was then concentrated to a red oil. Water was added and the solution was adjusted to pH 1 with concentrated hydrochloric acid. The product was extracted with diethylether. The organic layer was dried over magnesium sulfate and diethylether was evaporated under reduced pressure. The residue was dissolved in a small volume of methanol. The solution was treated with charcoal, filtered and water was added to the filtrate. The resulting precipitate was collected by filtration, washed with water and dried (79%). mp: 63-66° C., IR (KBr): υ: 3086 (C—H aromatic), 2976, 2931 (C—H aliphatic), 1693 (C=0) cm−1, Anal. (C11H11O2Cl) C, H. The mixture was then concentrated to a red oil Water was added The product was extracted with diethylether The organic layer was dried over magnesium sulfate and diethylether was evaporated under reduced pressure The residue was dissolved in a small volume of methanol The solution was treated with charcoal filtered water was added to the filtrate The resulting precipitate was collected by filtration washed with water dried (79%)