Benzaldehyde → 4-Piperidinone, 3,5-bis(phenylmethylene)-, hydrochloride

HRID 462254

Reaktionsgleichung

Reaktionsgleichung von HRID 462254
[ClH:1].[NH:2]1[CH2:7][CH2:6][C:5](=[O:8])[CH2:4][CH2:3]1.[CH:9](=O)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.Cl>C(O)C>[ClH:1].[CH:9](=[C:4]1[C:5](=[O:8])[C:6](=[CH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:7][NH:2][CH2:3]1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

Komponenten

5

Edukt 3

HCID 240BenzaldehydeHCID 313Hydrochloric AcidHCID 30848514-Piperidone hydrochloride

Produkt 1

HCID 3557494-Piperidinone, 3,5-bis(phenylmethylene)-, hydrochlorideAusbeute 94,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A stirred solution of 10 g of 4-piperidone, hydrochloride, hydrate and 14 g of benzaldehyde in 50 ml of ethanol is cooled to 10° C and treated dropwise with 25 ml of concentrated hydrochloric acid (temperature maintained at less than 25° C during the addition) and refluxed for 4 hours; the product begins to separate soon after refluxing begins. After standing at room temperature for about 16 hours, the resulting solid is filtered, washed with cold ethanol and with ether, and air-dried yielding 19.4 g of material, melting point 272°-274° C, dec.

Aufarbeitung

  1. temperaturemaintained at less than 25° C during the addition) and
  2. temperaturerefluxed for 4 hours
  3. customto separate soon
  4. temperatureafter refluxing
  5. filtrationthe resulting solid is filtered
  6. washwashed with cold ethanol and with ether
  7. customair-dried

Quellen und Nachweise

ORD-Eintrag
ord-2638860426694659ae38256e7d6e47d8
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04065617

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