tert-Butyl carbazate → Tert-butyl 2-(1-methylpiperidin-4-ylidene)hydrazinecarboxylate
Reaktionsgleichung
[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=O)[CH2:4][CH2:3]1.[C:9]([NH:16][NH2:17])([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10]>>[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=[N:17][NH:16][C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:4][CH2:3]1Komponenten
3
Versuchsvorschrift
A solution of 11.2 g (99.0 mmol) of 1-methyl-piperid-4-one and 13.0 g (100 mmol) of Boc-hydrazine in 150 mL of hexanes was refluxed for 30 minutes. The hot solution was dried over MgSO4, filtered, and allowed to cool. The resulting crystals were isolated and recrystallized from Et2O to provide 7.2 g of tert-butyl N′-(1-Methyl-piperidin-4-ylidene)-hydrazinecarboxylate as a white solid.
Aufarbeitung
- dry with materialThe hot solution was dried over MgSO4
- filtrationfiltered
- temperatureto cool
- customThe resulting crystals were isolated
- customrecrystallized from Et2O
Quellen und Nachweise
- ORD-Eintrag
- ord-bd36b320da88410b94f7e7655875b826
- Quelldatensatz
- uspto-grants-2009_04
- Patentnummer
- US07514458B2
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