反应 #3007855
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06171866B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A suspension of 24.6 g (200 mmol) o-anisidine M10, 20.8 g (220 mmol) chloroethyl methyl ether M11, 30.4 g (220 mmol) K2CO3 and 18.3 g (110 mmol) KI in 110 ml DMF was heated at 95° C. for 24 hours. DMF was evaporated, and the residue was digested with 100 ml CHCl3, filtered, and the precipitate washed with 2×50 ml CHCl3. The solvent was evaporated to give 41.2 g crude oil. This oil was purified by a plug packed with 184 g silica gel 100 with CHCl3/cyclohexane (1:1, v/v) as eluant, to afford 23.5 g pure product (yield: 65%). DMF was evaporated filtered the precipitate washed with 2×50 ml CHCl3 The solvent was evaporated to give 41.2 g crude oil This oil was purified by a plug
来源 ID: ord-2f5d5daa013a4bc1b544cea3c2debd7f