反応 #214784

反応方程式

1,2,5-trimethyl-β-oxo-3-pyrrolpropionitrile

toluene

phenylisocyanate

→

1,2,5-trimethyl-β-oxo-α-phenylcarbamoyl-3-pyrrolpropionitrile

溶媒

triethylamine

反応条件

後処理

1. 1
   温度warmed for 5 minutes on the steam cone until
2. 2
   workup.DISSOLUTIONall is dissolved
3. 3
   その他the precipitate formed
4. 4
   その他is collected
5. 5
   workup.ADDITIONthe solution added to the mixture of 3 ml of 5 N hydrochloric acid and 250 ml of water
6. 6
   その他The crude product formed
7. 7
   その他is collected
8. 8
   洗浄washed with water
9. 9
   workup.DISSOLUTIONdissolved in 5% aqueous sodium hydroxide
10. 10
    ろ過filtered
11. 11
    その他The precipitate is collected
12. 12
    洗浄washed with water
13. 13
    その他air-dried
14. 14
    その他recrystallized from ethanol

実験手順

The suspension of 1.0 g of 1,2,5-trimethyl-β-oxo-3-pyrrolpropionitrile, 40 ml of toluene and 0.7 g of triethylamine is treated with 0.75 g of phenylisocyanate and warmed for 5 minutes on the steam cone until all is dissolved. After standing overnight, the precipitate formed is collected, taken up in methanol, and the solution added to the mixture of 3 ml of 5 N hydrochloric acid and 250 ml of water. The crude product formed is collected, washed with water, dissolved in 5% aqueous sodium hydroxide, filtered, and the alkaline filtrate acidified with 5 N hydrochloric acid. The precipitate is collected, washed with water, air-dried and recrystallized from ethanol, to yield the 1,2,5-trimethyl-β-oxo-α-phenylcarbamoyl-3-pyrrolpropionitrile melting at 158°-160°.

出典