Lithium hydroxide, monohydrate → Di-tert-butyl 1-(1-acetylpiperidin-4-yl)hydrazine-1,2-dicarboxylate

HRID 44648Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 44648
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([N:10]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[N:11](C(=O)C2C=CC=CC=2)[C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].O.[OH-].[Li+]>O1CCCC1.O>[C:1]([N:4]1[CH2:5][CH2:6][CH:7]([N:10]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[NH:11][C:12]([O:14][C:15]([CH3:16])([CH3:17])[CH3:18])=[O:13])[CH2:8][CH2:9]1)(=[O:3])[CH3:2]

Komponenten

5

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 68934227Di-tert-butyl 1-(1-acetylpiperidin-4-yl)-2-benzoylhydrazine-1,2-dicarboxylate

Produkt 1

HCID 57444162Di-tert-butyl 1-(1-acetylpiperidin-4-yl)hydrazine-1,2-dicarboxylateAusbeute 89,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

45 g (0.1 mol) of di-tert-butyl 1-(1-acetylpiperidin-4-yl)-2-benzoylhydrazine-1,2-dicarboxylate were dissolved in 1 L of tetrahydrofuran and a solution of 5.8 g (0.14 mol) of lithium hydroxide monohydrate in 1 L of water were added. The mixture was stirred at room temperature for 16 hours, the tetrahydrofuran removed in vacuo and the aqueous layer extracted several times with dichloromethane. The organic phase was dried over sodium sulfate and evaporated to dryness, giving 32 g (84% yield) of the title compound.

Aufarbeitung

  1. customthe tetrahydrofuran removed in vacuo
  2. extractionthe aqueous layer extracted several times with dichloromethane
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-98a349149d954d3498b5555fe29534a9
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08541429B2

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