1-Piperazinecarboxylic acid, ethyl ester → HCID 21423023, Verbindung

HRID 259068Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 259068
[CH2:1]([O:3][C:4]([N:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)=[O:5])[CH3:2].CS(O[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])(=O)=O.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH2:1]([O:3][C:4]([N:6]1[CH2:7][CH2:8][N:9]([CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH3:17])[CH2:10][CH2:11]1)=[O:5])[CH3:2]

Komponenten

5

Edukt 3

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 10340Sodium CarbonateHCID 1477736462732-70-1

Produkt 1

HCID 21423023HCID 21423023, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

25.0 Grams of 1-ethoxycarbonylpiperazine, 43.0 grams of pentadecyl methylsulfonate, 250 ml. of ethanol, and 9.53 grams of sodium carbonate are combined and heated to gentle reflux. After refluxing for 6 hours, the mixture is filtered, and the solvents removed under reduced pressure. The residue is dissolved in a mixture of water and ethyl ether. The organic layer is separated, washed once with water, and dried over anhydrous magnesium sulfate and anhydrous sodium sulfate. The solvent is removed under reduced pressure to give 1-ethoxycarbonyl-4-pentadecylpiperazine.

Aufarbeitung

  1. temperatureheated to gentle reflux
  2. temperatureAfter refluxing for 6 hours
  3. filtrationthe mixture is filtered
  4. customthe solvents removed under reduced pressure
  5. dissolutionThe residue is dissolved in a mixture of water and ethyl ether
  6. customThe organic layer is separated
  7. washwashed once with water
  8. dry with materialdried over anhydrous magnesium sulfate and anhydrous sodium sulfate
  9. customThe solvent is removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-71f863436d834a46b2e0e2ae41f3ca0c
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04036828

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