反応 #214782

反応方程式

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

phenylisocyanate

→

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

溶媒

toluene

triethylamine

反応条件

後処理

1. 1
   workup.ADDITIONare added
2. 2
   温度The mixture is warmed for 5 minutes at the steam cone
3. 3
   ろ過It is filtered
4. 4
   その他The precipitate formed
5. 5
   その他is collected
6. 6
   workup.DISSOLUTIONdissolved in N aqueous sodium hydroxide
7. 7
   その他re-precipitated with 5 N hydrochloric acid
8. 8
   洗浄washed with water

実験手順

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°.

出典