Reaktion #1797958

Reaktionsgleichung

4-(3-chloropropoxy)-2-fluorobenzamide

1,3-dichloroacetone

→

4-(chloromethyl)-2-[4-(3-chloropropoxy)-2-fluorophenyl]-1,3-oxazole

Ausbeute 44.0%

Lösungsmittel

propionitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe mixture is then concentrated under vacuum
2. 2
   Waschenwashed with water
3. 3
   TrocknenThe organic phase is dried over magnesium sulfate
4. 4
   Einengenconcentrated under reduced pressure
5. 5
   SonstigeThe residue is purified by chromatography over silicagel (eluent: dichloromethane)

Vorschrift

A mixture of 4-(3-chloropropoxy)-2-fluorobenzamide i82 (0.41 g, 1.75 mmol, 1 eq) and 1,3-dichloroacetone (0.49 g, 3.85 mmol, 2.2 eq) in propionitrile (9 ml) is stirred at 100° C. for 60 h. The mixture is then concentrated under vacuum, taken up in dichloromethane, and washed with water. The organic phase is dried over magnesium sulfate and concentrated under reduced pressure. The residue is purified by chromatography over silicagel (eluent: dichloromethane) to afford 0.23 g of 4-(chloromethyl)-2-[4-(3-chloropropoxy)-2-fluorophenyl]-1,3-oxazole i84.

Quelle