Synfacts 2008(3): 0324-0324  
DOI: 10.1055/s-2008-1042670
Polymer-Supported Synthesis
© Georg Thieme Verlag Stuttgart · New York

Solid-Phase Synthesis of N-Aminodipeptides in High Optical Purity

Contributor(s):Yasuhiro Uozumi, Toshimasa Suzuka
A.-S. Felten, R. Vanderesse, N. Brosse, C. Didierjean, B. Jamart-Grégoire*
Nancy-Université, France
Solid Phase Synthesis of N-Aminodipeptides in High Optical Purity
Tetrahedron Lett.  2008,  49:  156-158  
Further Information

Publication History

Publication Date:
21 February 2008 (online)


Significance

A solid-phase synthesis of N-ami­nodipeptide derivatives via the Mitsunobu protocol was developed. Thus, the reaction of (S)-α-hydroxy acids 1 with a Wang resin using DIC followed by the deprotection of the resulting THP esters 2 gave the α-hydroxy esters 3. The Mitsunobu reaction of 3 with (S)-α-aminohydrazine phthalimide 4 afforded the polymer-supported esters 5. TFA-mediated cleavage of 5 gave the N-aminodipeptide derivatives 6a-j in 21-55% yield with excellent diastereomeric purity (>95% de).

Comment

Previously, Jamart-Grégoire and co-workes have reported the efficient synthesis of N-aminodipeptides via the solution-phase Mitsunobu reaction (N. Brosse, A. Grandeury, B. Jamart-Grégoire Tetrahedron Lett. 2002, 43, 2009). This report describes the first solid-phase application of the N-aminodipeptide synthesis via the Mitsunobu protocol. The absolute configuration of 6f was determined to be (S,R) by chemical correlation with the authentic 7f.