反応 #1993389

反応方程式

4H-quinolizin-4-one-3-carboxamide

→

3-cyano-4H-quinolizin-4-one

溶媒

phosphorus oxychloride

反応条件

後処理

1. 1
   温度was refluxed for one hour
2. 2
   濃縮The reaction mixture was concentrated under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue was dissolved in aqueous sodium bicarbonate solution
4. 4
   抽出The chloroform extract
5. 5
   洗浄was washed with water
6. 6
   乾燥dried over anhydrous magnesium sulfate
7. 7
   その他evaporated
8. 8
   その他The residue was chromatographed on silica gel (30 g)
9. 9
   洗浄eluting with chloroform-methanol (50:1)

実験手順

A mixture of 4H-quinolizin-4-one-3-carboxamide (1.0 g) and phosphorus oxychloride (50 ml) was refluxed for one hour. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in aqueous sodium bicarbonate solution and chloroform. The chloroform extract was washed with water, dried over anhydrous magnesium sulfate and then evaporated. The residue was chromatographed on silica gel (30 g) eluting with chloroform-methanol (50:1) to give 3-cyano-4H-quinolizin-4-one, which on recrystallization from ether gave crystals (800 mg), mp. 198°-200° C.

出典