Water → 1-Isopropyl-3,3,5,5-tetramethylpiperazine

HRID 2107954Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2107954
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH:7]([N:10]1[CH2:15][C:14]([CH3:17])([CH3:16])[NH:13][C:12]([CH3:19])([CH3:18])[C:11]1=O)([CH3:9])[CH3:8].O>O1CCCC1>[CH:7]([N:10]1[CH2:15][C:14]([CH3:17])([CH3:16])[NH:13][C:12]([CH3:19])([CH3:18])[CH2:11]1)([CH3:9])[CH3:8]

Komponenten

5

Edukt 3

HCID 962WaterHCID 125809921-Isopropyl-3,3,5,5-tetramethyl-2-piperazinoneHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 230449871-Isopropyl-3,3,5,5-tetramethylpiperazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

3.9 g (0.103 mol) of lithiumaluminium hydride are introduced into 100 ml of anhydrous tetrahydrofuran under a nitrogen atmosphere, while stirring and cooling. A solution of 19.8 g (0.1 mol) of 1-isopropyl-3,3,5,5-tetramethyl-2-piperazinone (obtainable, for example, in accordance with Synthesis 1981, page 40, or J. Organ. Chem., 45 (1980), 754-59) in 75 ml of anhydrous tetrahydrofuran is added dropwise at room temperature, whereupon the reaction temperature rises to 6020 C. The mixture is then stirred overnight at room temperature. After dropwise addition of about 10 ml of water, the mixture is subsequently stirred for 2 hours and the precipitate is then filtered off with suction. The filtrate is dried over potassium carbonate and concentrated in vacuo and the crude product which remains as a colourless oil is further processed without additional purification.

Aufarbeitung

  1. temperaturecooling
  2. customis added dropwise at room temperature, whereupon the reaction temperature
  3. stirringThe mixture is then stirred overnight at room temperature
  4. stirringthe mixture is subsequently stirred for 2 hours
  5. filtrationthe precipitate is then filtered off with suction
  6. dry with materialThe filtrate is dried over potassium carbonate
  7. concentrationconcentrated in vacuo
  8. customis further processed without additional purification

Quellen und Nachweise

ORD-Eintrag
ord-11165a5f4cae45b59dbfde76896cfbe6
Quelldatensatz
uspto-grants-1990_06
Patentnummer
US04937244

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