Cyclohexylpyrrolidinium hydrochloride salt → 1-Cyclohexylpyrrolidine

HRID 514645

Reaktionsgleichung

Reaktionsgleichung von HRID 514645
Cl.[CH:2]1([NH+:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1>O>[CH:2]1([N:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1

Komponenten

3

Edukt 1

HCID 131733292Cyclohexylpyrrolidinium hydrochloride salt

Produkt 1

HCID 1390641-Cyclohexylpyrrolidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

In some instances when some unreacted cyclohexanone is still in the reaction mixture, the product after hydrogenation was purified by adding 3M HCl solution to the mixture (after filtering out the palladium/carbon catalyst) and left to stir for 15-20 minutes. The resulting mixture was then extracted with diethyl ether to remove the cyclohexanone from the mixture and leaving behind the cyclohexylpyrrolidinium hydrochloride salt. The water layer containing cyclohexylpyrrolidinium hydrochloride salt is separated and then neutralized with NaOH solution to a pH of 9-10. The free cyclohexylpyrrolidine is extracted with ethyl acetate, dried over MgSO4 and concentrated on a rotary evaporator at reduced pressure to give the desired product free from any impurities.

Aufarbeitung

  1. customis separated
  2. extractionThe free cyclohexylpyrrolidine is extracted with ethyl acetate
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated on a rotary evaporator at reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-8d54c468fe694162aa87f9dd325baa01
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09108856B2

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