Methylamine → N-methyl-1-[1-(4-chlorophenyl)cyclobutyl]ethylamine
Reaktionsgleichung
[C:1]([C:4]1([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[CH2:7][CH2:6][CH2:5]1)(=O)[CH3:2].C(C1(C2C=CC(Cl)=C(Cl)C=2)CCC1)(=O)C.[CH3:30][NH2:31].[H][H]>C(O)C.[Pt]=O>[CH3:30][NH:31][CH:1]([C:4]1([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[CH2:7][CH2:6][CH2:5]1)[CH3:2]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
1Acetyl-1-(4-chlorophenyl)cyclobutane (61 g prepared in a similar manner to that described in Example 1 for 1-acetyl-1-(3,4-dichlorophenyl)cyclobutane, platinum oxide (0.75 g), 33% solution of methylamine in ethanol (60 g) and ethanol (30 ml) were charged into an autoclave. The autoclave was filled with hydrogen and maintained at about 60° C. and 20 bar pressure for ten hours. The reaction mixture was filtered through charcoal and the solids washed with absolute alcohol. The solvents were removed by evaporation and a sample of the residue (10 g) was shaken with 2M hydrochloric acid (50 ml) and ether (50 ml). The aqueous layer was basified and extracted with ether. The ether extract yielded a liquid on evaporation which was distilled (109° C./0.3 mm Hg) to give N-methyl-1-[1-(4-chlorophenyl)cyclobutyl]ethylamine (Formula I R1 =Me; R2 =H; R3 =Me; R4 =H; R5 =4-Cl and R6 =H).
Aufarbeitung
- additionwere charged into an autoclave
- wait20 bar pressure for ten hours
- filtrationThe reaction mixture was filtered through charcoal
- washthe solids washed with absolute alcohol
- customThe solvents were removed by evaporation
- extractionextracted with ether
- extractionThe ether extract
- customyielded a liquid
- customon evaporation which
- distillationwas distilled (109° C./0.3 mm Hg)
Quellen und Nachweise
- ORD-Eintrag
- ord-7b1ad4225d5040a18f70a582ee2ac020
- Quelldatensatz
- uspto-grants-1989_03
- Patentnummer
- US04814352
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