反应 #1474776
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05539112
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 2.15 g (9.39 mmol) of the resulting 2,4-difluoro-5-pivaloylaminophenol was dissolved in 40 ml of dichloromethane, 4.3 ml of 3,4-dihydro-2H-pyrane and 44 mg of camphorsulfonic acid were added and the mixture was stirred at room temperature for 4.3 hours. The reaction solution was added to a 5% aqueous solution of potassium carbonate and the mixture was extracted with chloroform. The organic layer was washed once with water and once with an aqueous saturated solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent Was distilled off under reduced pressure and the residue was triturated with n-hexane to give 2.51 g (85%) of 2,4-difluoro-5-pivaloylamino-O-(2-tetrahydropyranyl)phenol. the mixture was extracted with chloroform The organic layer was washed once with water and once with an aqueous saturated solution of sodium chloride dried over anhydrous magnesium sulfate The solvent Was distilled off under reduced pressure the residue was triturated with n-hexane
来源 ID: ord-fa13999c6a224c988d7a1716c5c528fa