Hydrochloric Acid → N-Acetyl-3,4-dimethoxyphenethylamine

HRID 2253610

Reaktionsgleichung

Reaktionsgleichung von HRID 2253610
[CH2:1]([NH2:13])[CH2:2][C:3]1[CH:12]=[CH:11][C:8]([O:9][CH3:10])=[C:5]([O:6][CH3:7])[CH:4]=1.[C:14](OC(=O)C)(=[O:16])[CH3:15].Cl>N1C=CC=CC=1>[C:14]([NH:13][CH2:1][CH2:2][C:3]1[CH:12]=[CH:11][C:8]([O:9][CH3:10])=[C:5]([O:6][CH3:7])[CH:4]=1)(=[O:16])[CH3:15]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 8421Homoveratrylamine

Produkt 1

HCID 80465N-Acetyl-3,4-dimethoxyphenethylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

After dissolving 5 g of homoveratrylamine in 20 ml of pyridine, 5.6 g of acetic anhydride was added and reacted at 65°-70° C. with stirring for 2 hours. The reaction mixture was poured into 150 ml of ice water and then made weakly acidic by adding 50 ml of a 6N aqueous hydrochloric acid solution. The resultant solution was extracted three times with 50 ml of chloroform. The extracted solution was combined, washed with an aqueous sodium hydrogen carbonate solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. Ether was added to the residue and precipitated crystals were filtered. N-acetylhomoveratrylamine having a melting point of 101°-102° C. was obtained as colorless crystals. The yield was 5.7 g.

Aufarbeitung

  1. additionwas added
  2. customreacted at 65°-70° C.
  3. extractionThe resultant solution was extracted three times with 50 ml of chloroform
  4. washwashed with an aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. additionEther was added to the residue
  8. customprecipitated crystals
  9. filtrationwere filtered

Quellen und Nachweise

ORD-Eintrag
ord-55778aa0a8aa43f48ab07dc4aa993ad6
Quelldatensatz
uspto-grants-1993_08
Patentnummer
US05232923

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