反应 #1869217

ord-568c9d6a32e34e1fa7c3768c361c2f53

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩concentrated in vacuo
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in xylene (10 ml)
  3. 3
    workup.STIRRINGThe resulting mixture was stirred for 18 h at 70° C
  4. 4
    workup.ADDITIONwas poured
  5. 5
    workup.STIRRINGinto stirred ice-cold water
  6. 6
    萃取extracted with ether (2×30 ml)
  7. 7
    干燥The ether layer was dried over sodium sulfate
  8. 8
    过滤filtered
  9. 9
    浓缩concentrated

实验过程

To a solution of 4-tert-butyl-2-methoxybenzenesulfonyl chloride (258 mg, 0.99 mmol) in DMF (6 ml) was added pyrrolidine (70 mg, 0.99 mmol) and the solution was stirred at ambient temperature for 30 minutes, and concentrated in vacuo. The residue was dissolved in xylene (10 ml) and then added to mixture of AlCl3 (525 mg, 3.39 mmol) in xylene (5 ml). The resulting mixture was stirred for 18 h at 70° C. After colling the mixture was poured into stirred ice-cold water, and extracted with ether (2×30 ml). The ether layer was dried over sodium sulfate, filtered and concentrated to give 120 mg of subtitle compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07498338B2uspto-grants-2009_03