Tetrahedron p. 6031 - 6044 (1993)
Update date:2022-08-04
Topics: Regioselectivity Column chromatography NMR spectroscopy Enantiomeric excess (ee) Deprotonation Intramolecular cyclization Nucleophilic addition Cyclopropanation Protecting group Diastereomers Stereoselectivity Chiral Auxiliary Lewis Acid Catalysis Ring Strain Organometallic Compounds Functionalized chloroenamines Aminocyclopropane synthesis
Butz
Vilsmaier
Morpholino-chlorotetrahydro-N-methyl-pyridine 4 reacted with Grignard reagents 5 or diorganyl-magnesium compounds 6 to give a mixture of azabicyclo[3.1.0]hexane diastereomers 10 and 11 besides the monocyclic ketones 12. The latter were obtained as the sole products from chloroenamine 4 and dimethylzinc 7a or lithium dimethylcopper 8a. Organolithium compounds 9a,c or Grignard reagents 5a-c in the presence of TMEDA transferred 4 exclusively to endo-morpholino isomers 10. exo-Amines 11 coulb be obtained with high stereoselectivity from 4 via the N,O-acetal 13 and by the substitution of the methoxy moiety by a Grignard reagent. 5. The stereochemical result of this substitution reaction can be explained by an intermediate complexation of the pyrrolidine N-atom in 13 by the Grignard reagent 5. An N-benzyl chloroenamine 14 instead of the N-methyl compound 4 showed a different reaction behavior with methylmagnesium bromide 5a leading only to endo-amine 15 which could be used as a precursor of the parent bicyclic system 16. The configurations of the bicyclic diamines 10, 11 and 15 were determined via 1H NMR data.
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Doi:10.1021/ja00073a057
(1993)Doi:10.1016/j.molstruc.2017.05.121
(2017)Doi:10.14233/ajchem.2014.16428
(2014)Doi:10.1021/jo00076a044
(1993)Doi:10.1016/S0040-4020(01)87973-4
(1993)Doi:10.1021/jm00077a007
(1993)