Reaktion #1765245

Reaktionsgleichung

chloroacetone

chloroacetone

6-methoxypyridin-3-ol

potassium carbonate

potassium carbonate

→

clear oil

Ausbeute 60.4%

1-[(6-methoxypyridin-3-yl)oxy]acetone

Ausbeute 60.4%

Lösungsmittel

acetone

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe mixture was concentrated in vacuo
2. 2
   workup.DISSOLUTIONThe residue was dissolved in Et2O
3. 3
   Waschenwashed with H2O, brine
4. 4
   Trocknendried with Na2SO4
5. 5
   FiltrationThe solution was filtered
6. 6
   Einengenconcentrated in vacuo

Vorschrift

A solution of chloroacetone (3.7 g) and potassium iodide (65 mg) in acetone (7 mL) was stirred at approximately 25° C. overnight. In a second reactor, 6-methoxypyridin-3-ol (4.0 g, mmol) and potassium carbonate (1.3 g, 10 mmol) in acetone (5 mL) was refluxed for 15 min., then ¼ of chloroacetone/KI solution was added followed by additional potassium carbonate (1.3 g). This was repeated three times more, then the reaction stirred at approximately 25° C. overnight. The mixture was concentrated in vacuo. The residue was dissolved in Et2O and washed with H2O, brine and dried with Na2SO4. The solution was filtered and concentrated in vacuo yielding 3.5 g of clear oil that was used without further purification. This material darkened on standing over time.

Quelle