Acetic Anhydride → Acetamide, N-[(1R)-2-(4-methoxyphenyl)-1-methylethyl]-

HRID 569294Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 569294
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH:10]([NH2:12])[CH3:11])=[CH:5][CH:4]=1.[C:13](OC(=O)C)(=[O:15])[CH3:14]>N1C=CC=CC=1>[C:13]([NH:12][C@H:10]([CH3:11])[CH2:9][C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)(=[O:15])[CH3:14]

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 31721(+-)-p-Methoxyamphetamine

Produkt 1

HCID 11769683Acetamide, N-[(1R)-2-(4-methoxyphenyl)-1-methylethyl]-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

In 6 ml of pyridine was dissolved 1.5 g of (-)-2-(p-methoxyphenyl)-1-methylethylamine ([α]D23 : -30.1° (c=1.2, methanol)), and after adding thereto 3 ml of acetic anhydride, the mixture was allowed to stand at room temperature for 1 hour. After distilling off the solvent, the residue was extracted with ethyl acetate. The ethyl acetate extract was washed with water, and dried over anhydrous sodium sulfate, and the solvent was distilled off and the crude crystals formed were recrystallized from a mixture of n-hexane and benzene to provide 1.8 g of (R)(+)-N-acetyl-2-(p-methoxyphenyl)-1-methylethylamine.

Aufarbeitung

  1. additionafter adding
  2. distillationAfter distilling off the solvent
  3. extractionthe residue was extracted with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. washwas washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off
  8. customthe crude crystals formed
  9. customwere recrystallized from a mixture of n-hexane and benzene

Quellen und Nachweise

ORD-Eintrag
ord-3734550b42de4d38bc1e22804a036c25
Quelldatensatz
uspto-grants-1988_03
Patentnummer
US04731478

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