반응 #214782

반응 방정식

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

phenylisocyanate

→

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

용매

toluene

triethylamine

반응 조건

후처리

1. 1
   workup.ADDITIONare added
2. 2
   온도The mixture is warmed for 5 minutes at the steam cone
3. 3
   여과It is filtered
4. 4
   기타The precipitate formed
5. 5
   기타is collected
6. 6
   workup.DISSOLUTIONdissolved in N aqueous sodium hydroxide
7. 7
   기타re-precipitated with 5 N hydrochloric acid
8. 8
   세척washed with water

실험 절차

To the suspension of 1.0 g of 1,3,5-trimethyl-β-oxo-2-pyrrolpropionitrile in 30 ml of dry toluene and 0.7 g of anhydrous triethylamine, 0.75 g of phenylisocyanate are added while stirring. The mixture is warmed for 5 minutes at the steam cone and allowed to stand at room temperature overnight. It is filtered, the residue taken up in methanol and the solution acidified with N hydrochloric acid. The precipitate formed is collected, dissolved in N aqueous sodium hydroxide, re-precipitated with 5 N hydrochloric acid and washed with water, to yield the 1,3,5-trimethyl-β-oxo-α-phenylcarbamoyl-2-pyrrolpropionitrile melting at 172°-174°.

출처