Reaktion #65081

Reaktionsgleichung

3-(4-chloro-5-ethylsulfonylamino-2-fluorophenyl)-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

potassium carbonate

dimethyl sulfate

→

objective product

Ausbeute 118.3%

3-(4-chloro-5-ethylsulfonylamino-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

Ausbeute 118.3%

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONAfter acetone was distilled off
2. 2
   workup.DISSOLUTIONthe reaction product was dissolved in ethyl acetate
3. 3
   Waschenwashed with water and saturated saline solution
4. 4
   Trocknendried over anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONThereafter the ethyl acetate was distilled off
6. 6
   Sonstigeto obtain a crude product
7. 7
   SonstigeThe crude product was recrystallized from chloroformdiethyl ether

Vorschrift

1.00 g (2.41 mmol) of 3-(4-chloro-5-ethylsulfonylamino-2-fluorophenyl)-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione was dissolved in 10 ml of acetone, and 0.17 g (1.20 mmol) of anhydrous potassium carbonate and 0.23 ml (2.41 mmol) of dimethyl sulfate were added thereto and the reaction was continued for 1.5 hours. After acetone was distilled off, the reaction product was dissolved in ethyl acetate, washed with water and saturated saline solution, and dried over anhydrous sodium sulfate. Thereafter the ethyl acetate was distilled off to obtain a crude product. The crude product was recrystallized from chloroformdiethyl ether, thereby obtaining 0.61 g of the objective product (yield: 59%) in the form of light yellow crystals.

Quelle