反应 #1392659
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US03966758
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A 21.5 g (0.25 mole) portion of 2-imidazolidinone in 150 ml of dimethylsulfoxide was treated with 34.5 g (0.25 mole) of potassium carbonate, 20 g (0.12 mole) of potassium iodide and 36.3 g (0.25 mole) of 3-fluorobenzyl chloride. The reaction mixture was heated with rapid stirring to 100° over 0.3 hours, held at 100° for 1.8 hours and poured with rapid stirring into 1.5 l of cold water. The aqueous mixture was extracted with 1.3 l of chloroform. The chloroform extract was washed with 500 ml of water, dried over magnesium sulfate overnight and filtered. The filtrate was concentrated to dryness to give 46 g (94%) of a light green semi-solid. The crude product was washed with 125 ml of ether, filtered and air dried to give 13.5 g (28%) of a white solid, m.p. 103°-105°. The reaction mixture was heated held at 100° for 1.8 hours poured The aqueous mixture was extracted with 1.3 l of chloroform The chloroform extract was washed with 500 ml of water dried over magnesium sulfate overnight filtered The filtrate was concentrated to dryness
来源 ID: ord-5887b4776cee4cc6a967e3a81f36a376