Reaktionsgleichung
[OH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.C1(=O)O[CH2:11][CH2:10][O:9]1.C([O-])([O-])=O.[K+].[K+].CN(C=O)C>C1(=O)OCCO1.O>[N:4]1[CH:5]=[CH:6][CH:7]=[C:2]([O:1][CH2:11][CH2:10][OH:9])[CH:3]=1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 86 °C
Versuchsvorschrift
3-hydroxypyridine (20.0 kg), ethylene carbonate (19.4 kg), K2CO3 (18.9 kg), and DMF (75.5 kg) were charged to a 400 L reactor and heated to 86° C. After 13H, an aliquot was taken. There was still some 3-hydroxypyridine left by GC so more ethylene carbonate (1.0 kg) was added. After 20H, the reaction was deemed complete. The reaction was cooled to 20° C., H2O (85 L) was slowly added to the 400 L reactor, and stirring continued for 30 min. The title compound was extracted with 35° C. CH2Cl2 (4×170 L) sending the CH2Cl2 extractions into the 1000 L portable tank. The aqueous layer was discarded, and the 400 L reactor was cleaned. The solution of the title compound in the 1000 L portable tank was transferred to the 400 L and distilled in the 400 L reactor sending the distillate to the 400 L receiver. Toluene (200 L) was added so the 400 L reactor and distilled sending the distillate to the 400 L receiver. The resulting oil was transferred to a 20 L glass bottle to produce 21.0 kg (72%) of the title compound of 100.0% GC purity.
Aufarbeitung
- additionwas added
- temperatureThe reaction was cooled to 20° C.
- extractionThe title compound was extracted with 35° C
- extractionthe CH2Cl2 extractions into the 1000 L portable tank
- distillationdistilled in the 400 L reactor
- additionToluene (200 L) was added so the 400 L reactor
- distillationdistilled
Quellen und Nachweise
- ORD-Eintrag
- ord-ffd687ac69c54711aaca5846f746f590
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08835439B2
Verknüpfte Notizen
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