Реакция #214784

Уравнение реакции

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

toluene

phenylisocyanate

→

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

Растворители

triethylamine

Условия реакции

Обработка

1. 1
   Температураwarmed for 5 minutes on the steam cone until
2. 2
   workup.DISSOLUTIONall is dissolved
3. 3
   Другоеthe precipitate formed
4. 4
   Другоеis 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
   ДругоеThe crude product formed
7. 7
   Другоеis collected
8. 8
   Промывкаwashed with water
9. 9
   workup.DISSOLUTIONdissolved in 5% aqueous sodium hydroxide
10. 10
    Фильтрацияfiltered
11. 11
    ДругоеThe precipitate is collected
12. 12
    Промывкаwashed with water
13. 13
    Другоеair-dried
14. 14
    Другоеrecrystallized from ethanol

Методика

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°.

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