Ethanol → Ethyl 4-decylpiperazine-1-carboxylate

HRID 259066Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 259066
CS(O[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])(=O)=O.[CH2:16]([O:18][C:19]([N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)=[O:20])[CH3:17].C(O)C.C(=O)([O-])[O-].[K+].[K+]>O.C(OCC)C>[CH2:16]([O:18][C:19]([N:21]1[CH2:22][CH2:23][N:24]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH2:25][CH2:26]1)=[O:20])[CH3:17]

Komponenten

7

Edukt 4

HCID 702EthanolHCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 11430Potassium CarbonateHCID 5235508Decyl methanesulfonate

Produkt 1

HCID 228932Ethyl 4-decylpiperazine-1-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

77.3 Grams of decyl methylsulfonate, 44.64 grams of 1-ethoxycarbonylpiperazine, 500 ml. of ethanol, and 39 grams of potassium carbonate are combined and refluxed for approximately 44 hours under a nitrogen atmosphere. After cooling to room temperature the residue is dissolved in a mixture of water and ethyl ether. The organic layer is separated, washed three times with portions of water and dried over anhydrous sodium sulfate. The solvents are removed under reduced pressure to give 1-ethoxycarbonyl-4-decylpiperazine.

Aufarbeitung

  1. temperaturerefluxed for approximately 44 hours under a nitrogen atmosphere
  2. customThe organic layer is separated
  3. washwashed three times with portions of water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvents are removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-2ab7a268626c4c259e68ae53ac0c746c
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04036828

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