反応 #5910

反応方程式

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

溶媒

water

dimethylformamide

ethyl acetate

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture is stirred for 12 hours at room temperature
2. 2
   workup.ADDITIONhas previously been added
3. 3
   乾燥dried over sodium sulfate
4. 4
   その他after evaporation
5. 5
   その他is purified
6. 6
   その他to give a colorless solid

実験手順

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.

出典