Reaktion #595523

Reaktionsgleichung

2-hydroxy-3,5-diiodobenzoic acid

dimethyl sulfate

acetone

→

solid

methyl 3,5-diiodo-2-methoxybenzoate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturat reflux for 16 h
3. 3
   Temperaturcooled
4. 4
   Einengenconcentrated
5. 5
   workup.DISSOLUTIONThe residue was dissolved in EtOAc
6. 6
   Waschenwashed with water, brine
7. 7
   Trocknendried (Na2SO4)
8. 8
   Filtrationfiltered
9. 9
   Einengenconcentrated

Vorschrift

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).

Quelle