N-(4-dimethylaminomethylphenylmethyl)acetamide → 4-Dimethylaminomethylbenzylamine

HRID 1595378Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1595378
[CH3:1][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH:12]C(=O)C)=[CH:7][CH:6]=1)[CH3:3]>Cl>[CH3:3][N:2]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][NH2:12])=[CH:7][CH:6]=1)[CH3:1]

Komponenten

3

Edukt 1

HCID 21703715N-(4-dimethylaminomethylphenylmethyl)acetamide

Produkt 1

HCID 1937144-DimethylaminomethylbenzylamineAusbeute 66,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

N-(4-Dimethylaminomethylphenylmethyl)acetamide (22 g) was dissolved in 4N hydrochloric acid (100 ml) and the mixture was refluxed under heating for 3 hr 40 min. The solvent was evaporated and ethyl acetate was added. The resulting crystals were collected by filtration. The obtained crystals were dissolved in water (40 ml) and potassium carbonate was added to saturation, and the mixture was extracted with chloroform. The extract was dried over anhydrous sodium sulfate and, after drying, the solvent was evaporated under reduced pressure to give the objective 4-(dimethylaminomethyl)phenylmethylamine (11.7 g), melting point 38-39° C.

Aufarbeitung

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 3 hr 40 min
  3. customThe solvent was evaporated
  4. additionethyl acetate was added
  5. filtrationThe resulting crystals were collected by filtration
  6. dissolutionThe obtained crystals were dissolved in water (40 ml)
  7. additionpotassium carbonate was added to saturation
  8. extractionthe mixture was extracted with chloroform
  9. dry with materialThe extract was dried over anhydrous sodium sulfate
  10. customafter drying
  11. customthe solvent was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7a3488afb51e4d84b089cd3ba7d292f4
Quelldatensatz
uspto-grants-2001_09
Patentnummer
US06288061B1

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