tert-Butyl carbazate → Tert-butyl 2-(1-methylpiperidin-4-ylidene)hydrazinecarboxylate

HRID 1350755Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1350755
[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]1

Komponenten

3

Edukt 2

HCID 70091tert-Butyl carbazateHCID 740491-Methyl-4-piperidone

Produkt 1

HCID 21097379Tert-butyl 2-(1-methylpiperidin-4-ylidene)hydrazinecarboxylateAusbeute 32 %

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

  1. dry with materialThe hot solution was dried over MgSO4
  2. filtrationfiltered
  3. temperatureto cool
  4. customThe resulting crystals were isolated
  5. customrecrystallized from Et2O

Quellen und Nachweise

ORD-Eintrag
ord-c0be285b2e644f6d8e94c21d0bfc47de
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07214802B2

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