反应 #1875634
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09051333B2
反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2-Bromo-1-(4-hydroxyphenyl)ethanone (2.90 g) and 2-(4-chlorophenoxy)acetamide (5.0 g) were added to N-methylpyrrolidone (5 ml), and the mixture was stirred at 100° C. under a nitrogen atmosphere. After being cooled to room temperature, ethyl acetate and a saturated sodium hydrogen carbonate aqueous solution were added to the reaction mixture and separated into layers. The organic layer was washed with water, dried over sodium sulfate, and then concentrated under reduced pressure. Sodium acetate (11.1 g) in DMF (20 ml) were added to the residue and then stirred at room temperature for 2 hours. The reaction mixture was diluted with ethyl acetate and the prepared insoluble matter was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1) and recrystallized from hexane-ethyl acetate to afford the title compound as a pale yellow powder (1.63 g). After being cooled to room temperature separated into layers The organic layer was washed with water dried over sodium sulfate concentrated under reduced pressure Sodium acetate (11.1 g) in DMF (20 ml) were added to the residue stirred at room temperature for 2 hours The reaction mixture was diluted with ethyl acetate the prepared insoluble matter was removed by filtration the filtrate was concentrated under reduced pressure The residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1→1:1) recrystallized from hexane-ethyl acetate
来源 ID: ord-cc2f89af174245109a2e201b321ee7d1