反応 #214768

反応方程式

1-methyl-β-oxo-2-pyrrolpropionitrile

p-fluorophenylisocyanate

→

1-methyl-β-oxo-α-(p-fluorophenylcarbamoyl)-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 on the steam cone until dissolution
3. 3
   その他It is evaporated on the steam cone
4. 4
   workup.ADDITIONthe solution poured into the mixture of 8 ml of 5 N hydrochloric acid and 300 ml of water
5. 5
   その他The precipitated crystals are collected
6. 6
   洗浄washed with water
7. 7
   その他dried
8. 8
   その他triturated with methanol

実験手順

To the suspension of 4.0 g of 1-methyl-β-oxo-2-pyrrolpropionitrile in 70 ml of toluene and 3.2 g of triethylamine, 3.7 g of p-fluorophenylisocyanate are added while stirring. The mixture is warmed on the steam cone until dissolution and the red-brown solution is allowed to stand overnight at room temperature. It is evaporated on the steam cone, the residue taken up in methanol and the solution poured into the mixture of 8 ml of 5 N hydrochloric acid and 300 ml of water. The precipitated crystals are collected, washed with water, dried, triturated with methanol and recrystalllized from ethyl acetate, to yield the 1-methyl-β-oxo-α-(p-fluorophenylcarbamoyl)-2-pyrrolpropionitrile melting at 198°-199°.

出典