反应 #1592785

ord-093b96b34b344a55ab55902bbbb8cf3f

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with water and brine
  2. 2
    干燥dried with MgSO4
  3. 3
    浓缩concentrated
  4. 4
    其他purified by silica gel column chromatography (20-100% EtOAc in heptane)

实验过程

To a solution of (4-bromo-2-fluoro-phenyl)methanamine (3 g, 14.7 mmol) in dichloromethane (50 mL) was added N,N-diisopropylethylamine (3.3 mL, 19.1 mmol), followed by phenylmethanesulfonyl chloride (3.3 g, 17.6 mmol) and the reaction was stirred at ambient temperature for 3 hours. The reaction was diluted with dichloromethane and washed with water and brine, dried with MgSO4, concentrated and purified by silica gel column chromatography (20-100% EtOAc in heptane) to give N-[(4-bromo-2-fluoro-phenyl)methyl]-1-phenyl-methanesulfonamide (4.22 g, 80% yield). LCMS (m/z) ES+ 358 [M+1]+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09216988B2uspto-grants-2015_12