Formaldehyde → 5-dimethylaminomethyl-5,6-dihydro-4H-thieno[2,3-b]thiopyran-4-one hydrochloride
Reaktionsgleichung
[S:1]1[C:5]2[S:6][CH2:7][CH2:8][C:9](=[O:10])[C:4]=2[CH:3]=[CH:2]1.[CH2:11]=O.[ClH:13].[CH3:14][NH:15][CH3:16]>C(O)(=O)C>[ClH:13].[CH3:14][N:15]([CH2:11][CH:8]1[CH2:7][S:6][C:5]2[S:1][CH:2]=[CH:3][C:4]=2[C:9]1=[O:10])[CH3:16]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
A mixture of 5,6-dihydrothieno[2,3-b]thiopyran-4-one (12.5 g, 0.074 mol), paraformaldehyde (7.5 g, 0.25 mol), dimethylamine-hydrochloride (40 g, 0.49 mol) and acetic acid (2 ml) was heated with stirring at 100° C. for 1 hour. After allowing to cool to room temperature, the solid was triturated with ethanol and the solid was collected on a filter to yield 16.3 g (83%) of the title compound. An analytical sample was prepared by crystallization from 95% ethanol and filtration through a pad of norite-ducco-supercel to yield product with mp 155°-157° C. Anal. Calc'd. for C10H13NOS2.HCl.
Aufarbeitung
- temperaturewas heated
- temperatureto cool to room temperature
- customthe solid was triturated with ethanol
- customthe solid was collected on
- filtrationa filter
Quellen und Nachweise
- ORD-Eintrag
- ord-fcf8cb3c8e5647a99d5a3dbc3049efd0
- Quelldatensatz
- uspto-grants-1991_07
- Patentnummer
- US05032598
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