反应 #44356

ord-e9a70226abf14d40b5da6d0b8f80ee6a

溶剂

反应条件

温度
20°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solvent was removed in vacuo
  2. 2
    workup.DISSOLUTIONthe residues dissolved in DCM
  3. 3
    萃取extracted with 2M sodium hydroxide (twice)
  4. 4
    洗涤The aqueous layers were washed with DCM
  5. 5
    萃取extracted with ethyl acetate (thrice)
  6. 6
    干燥These organic extracts were dried (MgSO4)
  7. 7
    其他evaporated

实验过程

Triphenylphosphine was added portionwise to a solution of 4-bromo-2-fluorobenzenesulfonyl chloride (8.44 g) in THF (30 ml) at 0° C. After 15 min water was added and the colourless solution was stirred at 20° C. for 18 h. The solvent was removed in vacuo, the residues dissolved in DCM and extracted with 2M sodium hydroxide (twice). The aqueous layers were washed with DCM, combined, acidified (4M HCl) and extracted with ethyl acetate (thrice). These organic extracts were dried (MgSO4) and evaporated to give the sub-title compound (5.89 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07737135B2uspto-grants-2010_06