反应 #11511

ord-f7ee27120d3e45df9a00b6188ab0a4c8

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤filtered over Celite
  2. 2
    其他the filtrate was evaporated to dryness under reduced pressure
  3. 3
    其他The residue was chromatographed on silica gel (230–400 mesh)
  4. 4
    洗涤eluted with 1% ethyl acetate in hexane
  5. 5
    其他to give 35 g (63%)

实验过程

Methyl 4-aminobenzoate (30.23 g, 200 mmol) was added to a mixture of iodine (60.91 g, 240 mmol) and silver sulfate (81.07 g, 260 mmol) in 1 L of ethanol at room temperature. The mixture was stirred at room temperature for 18 hours, filtered over Celite and the filtrate was evaporated to dryness under reduced pressure. The residue was chromatographed on silica gel (230–400 mesh) and eluted with 1% ethyl acetate in hexane to give 35 g (63%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07098231B2uspto-grants-2006_08