Benzaldehyde → 4-Piperidinone, 1-methyl-3,5-bis(phenylmethylene)-, hydrochloride

HRID 462252

Reaktionsgleichung

Reaktionsgleichung von HRID 462252
[CH3:1][N: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.[ClH:17]>C(O)C>[ClH:17].[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][N:2]([CH3:1])[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 740491-Methyl-4-piperidone

Produkt 1

HCID 3587084-Piperidinone, 1-methyl-3,5-bis(phenylmethylene)-, hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 57.0 g of 1-methyl-4-piperidone and 106.0 g of benzaldehyde in 400 ml of ethanol is cooled in an ice-bath and treated with hydrogen chloride gas until 250 g is absorbed. The solution is allowed to stand at room temperature for about 16 hours. The resulting solution is seeded, allowed to stand for about 16 hours at room temperature and the crystalline solid filtered on a sintered-glass funnel and washed with cold ethanol and then with ether. After drying in a desiccator, the solid (146 g) is digested in 400 ml of hot ethanol, cooled and filtered to give 120 g of product, melting point 242°-244° C, dec. Recrystallization of 11 g of this material from 35 ml of dimethylformamide gives 9.2 g of product, melting point 242°-244° C, dec.

Aufarbeitung

  1. customis absorbed
  2. waitto stand for about 16 hours at room temperature
  3. filtrationthe crystalline solid filtered on a sintered-glass funnel
  4. washwashed with cold ethanol
  5. customAfter drying in a desiccator
  6. temperaturecooled
  7. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-c503de4aa7884a33a74ca95625370b3b
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04065617

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