反应 #3467694
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06245761B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In a 25 ml flask, under a nitrogen atmosphere, 2-fluoro-5-bromobenzylbromide (755 mg, 2.82 mmol) was dissolved in methanol (10 ml). Methylamine (0.99 ml, 14.1 mmol) was added and the mixture was stirred at ambient temperature for about three hours. The progress of the reaction was monitored by thin layer chromatography. The solvents were removed by evaporation. The residue was partitioned between 1 M potassium carbonate and methylene chloride. The aqueous fraction was back extracted with methylene chloride. The organic fractions were combined and dried over sodium sulfate. The solvents were removed in vacuo. The title intermediate was further purified by liquid chromatography. The solvents were removed by evaporation The residue was partitioned between 1 M potassium carbonate and methylene chloride The aqueous fraction was back extracted with methylene chloride dried over sodium sulfate The solvents were removed in vacuo The title intermediate was further purified by liquid chromatography
来源 ID: ord-78498e19d24d4d07a5450b17c2b49d34