N-(4-Morpholinomethylphenylmethyl)acetamide hydrochloride → [4-(Morpholin-4-ylmethyl)phenyl]methanamine

HRID 1595375Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1595375
Cl.[O:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][NH:16]C(=O)C)=[CH:11][CH:10]=2)[CH2:4][CH2:3]1>Cl>[O:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][NH2:16])=[CH:11][CH:10]=2)[CH2:4][CH2:3]1

Komponenten

3

Edukt 1

HCID 21703892N-(4-Morpholinomethylphenylmethyl)acetamide hydrochloride

Produkt 1

HCID 2795501[4-(Morpholin-4-ylmethyl)phenyl]methanamineAusbeute 84,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

N-(4-Morpholinomethylphenylmethyl)acetamide hydrochloride (28.4 g) was dissolved in 4N hydrochloric acid (114 ml) and the mixture was refluxed under heating for 3 hr 15 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-(morpholinomethyl)phenylmethylamine (17.4 g), melting point 47-49° C.

Aufarbeitung

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 3 hr 15 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-e6392a97e6fb4e04b10839553d0aeb70
Quelldatensatz
uspto-grants-2001_09
Patentnummer
US06288061B1

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