反应 #2112489
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07759366B2
反应条件: temp:5.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1.3 g of tert-butyl (2-hydroxymethylphenyl)carbamate were dissolved in 20 ml of dichloromethane; at 5° C., a solution of 630 mg of phosphorus tribromide in 5 ml of DCM was then added dropwise. The reaction mixture was subsequently stirred at 5° C. for 2 h. For workup, the mixture was admixed cautiously with solid sodium hydrogencarbonate and 1 ml of water, stirred at 5° C. for 30 min, filtered through a cartridge and concentrated under reduced pressure. tert-Butyl (2-bromomethylphenyl)carbamate was obtained in a 67% yield. 1H NMR: 8.71, s, 1H, 7.45, d, 1H, 7.42, d, 1H, 7.3, t, 1H, 7.1, t, 1H; 4.78, 2, 2H, 1.45, s, 9H. stirred at 5° C. for 30 min filtered through a cartridge concentrated under reduced pressure
来源 ID: ord-4a75e1f2dcbc4049b4d64bd55035c30f