Reaktion #1722224

Reaktionsgleichung

benzoxazinone

potassium carbonate

DMF

→

2-(3-Cyanophenyl)-3,4-dihydro-2H-1,4-benzoxazin-3-one

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with ethyl acetate (3×150 mL)
2. 2
   WaschenThe combined organic extracts were washed with brine (2×100 mL)
3. 3
   Trocknendried with magnesium sulfate
4. 4
   Filtrationfiltered
5. 5
   Sonstigeevaporated in vacuo
6. 6
   SonstigeThe residue was purified on a silica gel column
7. 7
   Wascheneluted with 25% ethyl acetate in dichloromethane
8. 8
   SonstigeThe product (I1) was isolated 0.48 g (46%) as a light orange solid

Vorschrift

To the benzoxazinone (I6) (1.38 g, 4.17 mmol) in DMF (5 mL) was added potassium carbonate (1.40 g, 10.1 mmol), and the solution was stirred at room temperature for 1 hour. The solution was diluted with water and extracted with ethyl acetate (3×150 mL). The combined organic extracts were washed with brine (2×100 mL), dried with magnesium sulfate filtered, and evaporated in vacuo. The residue was purified on a silica gel column eluted with 25% ethyl acetate in dichloromethane. The product (I1) was isolated 0.48 g (46%) as a light orange solid.

Quelle