反応 #94066

反応方程式

Dicyclohexylcarbodiimide

3-acetylthio-2-carbamoylmethylpropanoic acid

→

3-Acetylthio-2-cyanomethylpropanoic acid

溶媒

pyridine

反応条件

後処理

1. 1
   ろ過the precipitate is filtered off
2. 2
   濃縮the filtrate is concentrated to dryness
3. 3
   workup.DISSOLUTIONthe residue is dissolved in ethyl acetate
4. 4
   抽出extracted with saturated aqueous bicarbonate
5. 5
   抽出extracted with ethyl acetate
6. 6
   その他This organic layer is dried
7. 7
   濃縮concentrated to dryness
8. 8
   その他The residue, 3-acetylthio-2-cyanomethylpropanoic acid is crystallized from ether-hexane, m.p. 110°-112°

実験手順

Dicyclohexylcarbodiimide (1.03 g.) is added to a solution of 3-acetylthio-2-carbamoylmethylpropanoic acid (1.02 g.) in pyridine (18 ml.). After five hours stirring at room temperature, the precipitate is filtered off and the filtrate is concentrated to dryness, the residue is dissolved in ethyl acetate and extracted with saturated aqueous bicarbonate. The aqueous phase is acidified and extracted with ethyl acetate. This organic layer is dried and concentrated to dryness. The residue, 3-acetylthio-2-cyanomethylpropanoic acid is crystallized from ether-hexane, m.p. 110°-112°.

出典