反应 #1973967

ord-55c8af9959c648fb8a25c335346d88b6

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度at reflux for 16 h
  3. 3
    温度cooled
  4. 4
    浓缩concentrated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in EtOAc
  6. 6
    洗涤washed with water, brine
  7. 7
    干燥dried (Na2SO4)
  8. 8
    过滤filtered
  9. 9
    浓缩concentrated

实验过程

A mixture of 2-hydroxy-3,5-diiodobenzoic acid (3.9 g, 10.0 mmol) potassium carbonate (4.15 g, 30.0 mmol) and dimethyl sulfate (2.77 g, 22.0 mmol) in acetone (33 ml) was heated at reflux for 16 h, cooled and concentrated. The residue was dissolved in EtOAc and washed with water, brine, dried (Na2SO4), filtered and concentrated to give an off-white solid (4.2 g, quantitative yield).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08501238B2uspto-grants-2013_08