Reaktion #2495512

Reaktionsgleichung

(2S)-7-hydroxy-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

phosphorus oxychloride

→

(2S)-7-chloro-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

Lösungsmittel

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONare added at room temperature and under an argon atmosphere
2. 2
   TemperaturAfter cooling
3. 3
   Sonstigethe reaction mixture is dry
4. 4
   Sonstigeevaporated under reduced pressure
5. 5
   workup.ADDITIONOn the obtained mixture, 32% soda is added up to a pH=6
6. 6
   SonstigeThe organic phase is then separated
7. 7
   Sonstigedried on magnesium sulphate
8. 8
   Filtrationfiltered
9. 9
   Einengenconcentrated under reduced pressure in order

Vorschrift

To a suspension of 5.6 g of (2S)-7-hydroxy-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one in 100 mL of 1,2-dichloroethane, are added at room temperature and under an argon atmosphere, 11 mL of phosphorus oxychloride. The resulting mixture is then heated to 70° C. After two hours of stirring and after monitoring with LC/MS, the reaction is completed. After cooling, the reaction mixture is dry evaporated under reduced pressure. The obtained residue is taken up with 5 mL of cold water and 200 mL of ethyl acetate. On the obtained mixture, 32% soda is added up to a pH=6. The organic phase is then separated and then dried on magnesium sulphate, filtered and concentrated under reduced pressure in order to obtain 6 g of (2S)-7-chloro-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one including the following characteristics:

Quelle