卢立康唑杂质1

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

实验步骤: (S)-2-Chloro-(2′,4′-dichlorophenyl)-1-ethanol (4 g, 17.74 mmol) was dissolved in 100 mL of anhydrous acetone (4 Å molecular sieves). The solution was flushed with nitrogen, and NaI (12.75 g, 85.10 mmol) was added to the solution and the solution refluxed for 3.5 hours under nitrogen. Upon cooling to room temperature, the solution was poured into about 320 mL of hexanes/ethyl acetate (3:1), with stirring. The solution was then filtered to remove excess NaI which had precipitated. The filtrate was evaporated to dryness in vacuo to yield a yellow oil. The oil was decanted, the residue treated with ether, and the ether washings decanted from the solid NaI. The ether solutions were combined and evaporated to dryness. Upon removal of ether, the product was obtained as a yellow crystalline solid. Yield: 4.70 g (84%). was added to the solution the solution refluxed for 3.5 hours under nitrogen The solution was then filtered to remove excess NaI which had precipitated The filtrate was evaporated to dryness in vacuo to yield a yellow oil The oil was decanted the residue treated with ether the ether washings decanted from the solid NaI evaporated to dryness Upon removal of ether the product was obtained as a yellow crystalline solid