Phosphorus sulfide (P2S5) → 2-(Thiophen-2-yl)ethanethioamide
Reaktionsgleichung
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][C:7]([NH2:9])=O.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:11]>C1COCC1>[CH:4]1[CH:3]=[C:2]([CH2:6][C:7]([NH2:9])=[S:11])[S:1][CH:5]=1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a solution in THF (200 mL) of 2-thiopheneacetamide (4.04 g, 28.6 mmol), prepared as in step 1, was added P4S10 (12,7 g, 28.6 mmol), and the vigorously stirred reaction mixture was placed in a Bransonic 221 bath and irradiated with ultrasound for 30 min. The reaction mixture was filtered and the tiltrate was concentrated in vacuo. The crude product was taken up in CH2Cl2 and decanted from the solid residue. Pure 2-thiophenethioacetamide (2.45 g, 54% yield) was obtained by chromatography on silica gel (CH2Cl2).
Aufarbeitung
- customthe vigorously stirred reaction mixture
- customirradiated with ultrasound for 30 min
- filtrationThe reaction mixture was filtered
- concentrationthe tiltrate was concentrated in vacuo
- customdecanted from the solid residue
Quellen und Nachweise
- ORD-Eintrag
- ord-1a3a301158814011a8b1f5c2bda94702
- Quelldatensatz
- uspto-grants-1997_04
- Patentnummer
- US05616596
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