Triethylamine → HCID 13458595, Verbindung

HRID 1248259Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1248259
[Cl:1][CH2:2][C:3](=[O:8])[CH2:4][CH2:5][CH2:6][CH3:7].[CH2:9]([N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1)[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].C(N(CC)CC)C>CCOCC>[ClH:1].[ClH:1].[CH2:9]([N:15]1[CH2:16][CH2:17][N:18]([CH2:2][C:3](=[O:8])[CH2:4][CH2:5][CH2:6][CH3:7])[CH2:19][CH2:20]1)[CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 2665711-chlorohexan-2-oneHCID 27365131-Hexylpiperazine

Produkt 1

HCID 13458595HCID 13458595, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

A solution of 8.5 g (0.07 mole) of 1-chloro-2-hexanone in 25 ml of ether was added dropwise to a mixture of 8.5 g (0.05 mole) of a n-hexyl piperazine and 10 g (0.1 mole) of triethylamine in 50 ml of ether. Addition was completed in 1 hour and the reaction mixture was stirred for 48 hours. The reaction mixture was filtered and the solvent was removed. The residue was dissolved in water, basified with 50% NaOH and extracted into toluene. The toluene was evaporated and the residue was treated with a saturated solution of HCl in isopropanol. The salt was filtered and crystallized twice from isopropanol to yield 6.2 g with a melting point of 190°-192° C.

Aufarbeitung

  1. additionAddition
  2. filtrationThe reaction mixture was filtered
  3. customthe solvent was removed
  4. dissolutionThe residue was dissolved in water
  5. extractionextracted into toluene
  6. customThe toluene was evaporated
  7. additionthe residue was treated with a saturated solution of HCl in isopropanol
  8. filtrationThe salt was filtered
  9. customcrystallized twice from isopropanol
  10. customto yield 6.2 g with a melting point of 190°-192° C.

Quellen und Nachweise

ORD-Eintrag
ord-5556700a5d6f43bdb829668a4c04778f
Quelldatensatz
uspto-grants-1985_06
Patentnummer
US04523014

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