Reaktion #5910

Reaktionsgleichung

orthophosphoric acid

sodium hydride

3-pyrazolyl-2-(N,N-dimethylaminooxycarbonyl)-phenol

2-methylsulfonyl-4,6-dimethoxypyrimidine

→

6-Pyrazolyl-2-(4,6-dimethoxypyrimidin-2-yloxy)-1-(N,N-dimethylaminooxycarbonyl)-benzene

Lösungsmittel

water

dimethylformamide

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture is stirred for 12 hours at room temperature
2. 2
   workup.ADDITIONhas previously been added
3. 3
   Trocknendried over sodium sulfate
4. 4
   Sonstigeafter evaporation
5. 5
   Sonstigeis purified
6. 6
   Sonstigeto give a colorless solid

Vorschrift

At 10° C., 0.30 g (0.01 mol) of sodium hydride (80% strength) is added to a solution of 2.47 g (10 mmol) of 3-pyrazolyl-2-(N,N-dimethylaminooxycarbonyl)-phenol in 25 ml of anhydrous dimethylformamide, and the reaction mixture is stirred for 3 hours at 30° C. 2.18 g (0.01 mol) of 2-methylsulfonyl-4,6-dimethoxypyrimidine is added and the mixture is stirred for 12 hours at room temperature. The reaction mixture is introduced into 500 ml of water to which 2.5 ml of orthophosphoric acid has previously been added. The oil which separates out is taken up in ethyl acetate and dried over sodium sulfate. The greasy residue remaining after evaporation is purified to give a colorless solid.

Quelle