N-Methylephedrine → Metamfepramone

HRID 1721533

Reaktionsgleichung

Reaktionsgleichung von HRID 1721533
[CH3:1][CH:2]([N:11]([CH3:13])[CH3:12])[CH:3]([OH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.IC1C=CC=CC=1C(O)=O>CS(C)=O.C([O-])(O)=O.[Na+]>[CH3:12][N:11]([CH3:13])[CH:2]([CH3:1])[C:3]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[O:10]

Komponenten

5

Edukt 2

HCID 4374N-MethylephedrineHCID 69412-Iodobenzoic acid

Produkt 1

HCID 71872MetamfepramoneAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 516892Sodium BicarbonateLösungsmittel

Versuchsvorschrift

N-Methylephedrine (500 mg, 2.79 mmol) was added to a solution of o-iodobenzoic acid I (7.8 g; 27.9 mmol) in DMSO (55 ml). After 48 hours the solution was diluted with NaHCO3 (2.5%, 30 ml) and extracted with ethyl acetate (3×10 ml). The combined organic layers were washed with water (2×5 ml), dried over sodium sulfate and evaporated to dryness under vacuum. The residue was purified by distillation to give 460 mg (92%) of 2-dimethylamino-1-phenyl-propan-1-one (boiling at 113°-117° C./12 mm).

Aufarbeitung

  1. extractionextracted with ethyl acetate (3×10 ml)
  2. washThe combined organic layers were washed with water (2×5 ml)
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness under vacuum
  5. distillationThe residue was purified by distillation

Quellen und Nachweise

ORD-Eintrag
ord-23aa75153c324d239afd01507e1b0edb
Quelldatensatz
uspto-grants-1996_04
Patentnummer
US05510538

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