反応 #1973967

反応方程式

2-hydroxy-3,5-diiodobenzoic acid

dimethyl sulfate

acetone

→

solid

methyl 3,5-diiodo-2-methoxybenzoate

反応条件

後処理

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

実験手順

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).

出典