Sodium Hydroxide → Piperazin-1-ylpropanol

HRID 80738

Reaktionsgleichung

Reaktionsgleichung von HRID 80738
C(OC([N:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][CH2:14][OH:15])[CH2:8][CH2:7]1)=O)C.[OH-].[Na+]>C(O)C>[OH:15][CH2:14][CH2:13][CH2:12][N:9]1[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]1

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 232657Ethyl 4-(3-hydroxypropyl)piperazine-1-carboxylate

Produkt 1

HCID 79207Piperazin-1-ylpropanolAusbeute 80,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

4-(3-hydroxypropyl)piperazinylcarboxylic acid ethyl ester (14.06 g, 65.09 mmol), 10% sodium hydroxide aqueous solution (150 mL) and ethanol (150 mL) were placed in a 500 mL round bottom flask, heated for refluxing and stirred overnight. The reaction was cooled down to room temperature, distilled under a reduced pressure to remove the solvent to obtain a light yellow oily substance, which was added with 200 mL saturated saline, and the resulting mixture was extracted with dichloromethane (5×200 mL), dried (Na2SO4), filtered, concentrated to obtain a light yellow oily substance, 7.56 g, yield 80.7%, which was directly used in the next step of reaction.

Aufarbeitung

  1. temperatureheated
  2. temperaturefor refluxing
  3. distillationdistilled under a reduced pressure
  4. customto remove the solvent
  5. customto obtain a light yellow oily substance, which
  6. additionwas added with 200 mL saturated saline
  7. extractionthe resulting mixture was extracted with dichloromethane (5×200 mL)
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customto obtain a light yellow oily substance, 7.56 g, yield 80.7%, which
  12. customwas directly used in the next step of reaction

Quellen und Nachweise

ORD-Eintrag
ord-d1c7ed72bc8e4c1bad9456339f5a2a07
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846678B2

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