반응 #1722224

반응 방정식

benzoxazinone

potassium carbonate

DMF

→

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

용매

water

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate (3×150 mL)
2. 2
   세척The combined organic extracts were washed with brine (2×100 mL)
3. 3
   건조dried with magnesium sulfate
4. 4
   여과filtered
5. 5
   기타evaporated in vacuo
6. 6
   기타The residue was purified on a silica gel column
7. 7
   세척eluted with 25% ethyl acetate in dichloromethane
8. 8
   기타The product (I1) was isolated 0.48 g (46%) as a light orange solid

실험 절차

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.

출처