Reaktionsgleichung
[O:1]1[CH2:6][CH2:5][N:4]([CH2:7][CH2:8][NH:9][C:10](=[S:13])[NH:11][NH2:12])[CH2:3][CH2:2]1.[C:14]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=1)(=O)[CH3:15].C(O)C>C(O)(=O)C>[O:1]1[CH2:2][CH2:3][N:4]([CH2:7][CH2:8][NH:9][C:10](=[S:13])[NH:11][N:12]=[C:14]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=2)[CH3:15])[CH2:5][CH2:6]1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A mixture of 6.00 g (0.0294 mole) of 4-(2-morpholinoethyl)thiosemicarbazide, 3.91 g (0.0323 mole) of 2-acetylpyridine, 20 mL of 95% ethanol, and 0.4 mL of glacial acetic acid was heated under reflux for 1.25 hours. The mixture then stood overnight at room temperature. Colourless crystals were collected and recrystallised from 40 mL of 95% ethanol; yield 7.81 g (86%) of pale yellow crystals of 2-acetylpryridine 4-(2-morpholinoethyl)thiosemicarbazone, mp 167.5°-169° C.
Aufarbeitung
- temperaturewas heated
- temperatureunder reflux for 1.25 hours
- customColourless crystals were collected
- customrecrystallised from 40 mL of 95% ethanol
Quellen und Nachweise
- ORD-Eintrag
- ord-1146570031294c70b5319c308ba10868
- Quelldatensatz
- uspto-grants-1988_07
- Patentnummer
- US04758572
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