Dicyclohexylcarbodiimide → HCID 20344450、化合物
反応式
C1(N=C=NC2CCCCC2)CCCCC1.[C:16]([S:19][CH2:20][CH:21]([CH2:25][C:26](=O)[NH2:27])[C:22]([OH:24])=[O:23])(=[O:18])[CH3:17]>N1C=CC=CC=1>[C:16]([S:19][CH2:20][CH:21]([CH2:25][C:26]#[N:27])[C:22]([OH:24])=[O:23])(=[O:18])[CH3:17]参加物
4
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 5 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°.
後処理
- filtrationthe precipitate is filtered off
- concentrationthe filtrate is concentrated to dryness
- dissolutionthe residue is dissolved in ethyl acetate
- extractionextracted with saturated aqueous bicarbonate
- extractionextracted with ethyl acetate
- customThis organic layer is dried
- concentrationconcentrated to dryness
- customThe residue, 3-acetylthio-2-cyanomethylpropanoic acid is crystallized from ether-hexane, m.p. 110°-112°
出典と根拠
- ORDレコード
- ord-83eb5f78a5a845ebb43a934c66ccec28
- 出典データセット
- uspto-grants-1978_05
- 特許番号
- US04091024
反応ノート
読み込み中…