反応 #214777

反応方程式

1-ethyl-β-oxo-2-pyrrolpropionitrile

toluene

phenylisocyanate

→

1-ethyl-β-oxo-α-phenylcarbamoyl-2-pyrrolpropionitrile

溶媒

triethylamine

反応条件

後処理

1. 1
   その他evaporated
2. 2
   workup.DISSOLUTIONthe residue dissolved in methanol
3. 3
   workup.ADDITIONThe solution is poured into 300 ml of water containing 5 ml of 5 N hydrochloric acid
4. 4
   その他the precipitate is collected
5. 5
   workup.DISSOLUTIONIt is dissolved in 5% aqueous sodium hydroxide
6. 6
   ろ過the solution filtered
7. 7
   その他the filtrate re-acidified, the solids collected
8. 8
   洗浄washed with water
9. 9
   その他dried
10. 10
    その他recrystallized from ethanol

実験手順

The mixture of 2.1 g of 1-ethyl-β-oxo-2-pyrrolpropionitrile, 25 ml of toluene and 1.6 g of triethylamine is treated with 1.6 g of phenylisocyanate while stirring. It is allowed to stand overnight at room temperature, evaporated and the residue dissolved in methanol. The solution is poured into 300 ml of water containing 5 ml of 5 N hydrochloric acid and the precipitate is collected. It is dissolved in 5% aqueous sodium hydroxide, the solution filtered, the filtrate re-acidified, the solids collected, washed with water, dried and recrystallized from ethanol, to yield the 1-ethyl-β-oxo-α-phenylcarbamoyl-2-pyrrolpropionitrile melting at 144°-145°.

出典