Реакция #1973967

ord-55c8af9959c648fb8a25c335346d88b6

Уравнение реакции

O=C(O)c1cc(I)cc(I)c1O
2-hydroxy-3,5-diiodobenzoic acid
COS(=O)(=O)OC
dimethyl sulfate
CC(C)=O
acetone
COC(=O)c1cc(I)cc(I)c1OC
solid
COC(=O)c1cc(I)cc(I)c1OC
methyl 3,5-diiodo-2-methoxybenzoate

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas heated
  2. 2
    Температураat reflux for 16 h
  3. 3
    Температураcooled
  4. 4
    Концентрированиеconcentrated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in EtOAc
  6. 6
    Промывкаwashed with water, brine
  7. 7
    Сушкаdried (Na2SO4)
  8. 8
    Фильтрацияfiltered
  9. 9
    Концентрированиеconcentrated

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08501238B2uspto-grants-2013_08