反应 #1710215
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05695737
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 40.1 g (310 mmol) of 2,4-dimethyl-4-hydroxymethyl-2-oxazoline (J. Nys and J. Libeer, Bull. Soco Chim. Belg., 65, 377 (1956)) and 85.5 g (326 mmol) of triphenylphosphine in 400 ml of dichloromethane is mixed at 0° C. in portions with 58.0 g (326 mmol) of N-bromosuccinimide and then stirred overnight at room temperature. The solution is concentrated by evaporation and the residue is pulverized with tert-butyl methyl ether. A precipitate develops, which is separated and washed with tert-butyl methyl ether. The combined filtrates are subjected to a fractionated distillation at normal pressure, and first the solvent is drawn off and then the title compound is distilled at an oil bath temperature of 200° C. The solution is concentrated by evaporation which is separated washed with tert-butyl methyl ether The combined filtrates are subjected to a fractionated distillation at normal pressure the title compound is distilled at an oil bath temperature of 200° C.
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