CRYSTAL STRUCTURE OF PNEUMOCYSTIS CARINII DIHYDROFOLATE REDUCTASE COFACTOR COMPLEX WITH TAB, A POTENT, PC-SELECTIVE ANTIFOLATE

N. Galitsky1, V. Cody1, D. Rak1, J.R. Luft1, W. Pangborn1, S.F. Queener2 M.F.G. Stevens3, C. Laughton3, and D. Chan3

1Hauptman-Woodward Medical Research Institute, Inc., 73 High St., Buffalo, New York 14203, USA
2Department of Pharmacology and Toxicology, Indiana University, Indianapolis, IN 46202, USA.
3University of Nottingham, Nottingham, UK NG7 2RD

Keywords: Dihydrofolate reductase, Pneumocystis carinii, antifolate, selectivity, structure-based drug design

To treat the pneumonia caused by opportunistic infectious agents, a major cause of mortality among patients with AIDS, the design of antifolate agents with selectivity against dihydrofolate reductase (DHFR) from Pneumocystis carinii (pc) has been the focus of many antifolate synthetic studies1. As part of our program to study inhibitor-bound DHFR complexes, we report the crystal structure determination of the ternary complex of pcDHFR with NADPH and 2,4-diamino-5-[3-[2-(acetyloxy)ethyl]-3-benzyltriazen-1-yl]-4-chlorophenyl]-6-ethylpyrimi- dine (TAB), one of the most potent and pcDHFR selective antifolates reported. The IC50 for pcDHFR is 0.17 mM with a selectivity index of 114 against rat liver DHFR2. Data were collected at room temperature on an RaxisIIc area detector system to 2.1A resolution for the monoclinic P21 crystals ( a = 37.481, b = 43.137, c = 61.266 A,b = 94.74o) and refined to R = 0.204. Analysis of the difference electron density indicate more than one conformer for TAB in the active site of pcDHFR. The 2,4-diaminopyrimidine ring interacts with Glu-32 in the same manner as other antifolates3 and the p-chlorophenyl ring torsion angle is near 60o. There are two alternate conformers for the 3'-benzyltriazenyl group in which the benzyl and acetoxy groups switch places. One conformer places the benzyl ring in a hydrophobic pocket between Phe-36 and Phe-69, with the acetyloxy group near Lys-30, and the second orientation positions the benzyl group near Ile-33, Pro-66 and Phe-69, with the acetoxyl group near Lys-37. While the benzyl ring occupies hydrophobic pockets in both orientations, there are no direct hydrogen bonds involving the keto function of the acetyl group, except through water mediation. Modeling studies of the binding interactions in the DHFR active site using molecular dynamics simulations were also carried out. These data showed four low energy binding models of which only two are in close agreement with this crystal structure determination. Comparison of structures of both human and pcDHFR suggest that the increased affinity for pcDHFR could result from sequence changes in the active site region. For example, interactions made by Lys-30, Ile-33, Lys-37 and Phe-69 with TAB in pcDHFR are replaced by Arg-28, Phe-31, Gln-35 and Asn-64 in the human structure. These changes, if mimicked in the rat liver enzyme, could play a key role in enhancing pcDHFR selectivity of this antifolate.

(Supported by GM-51670 (VC) and N01-AI-35171 (SFQ)).

1. S.F. Queener, J. Med. Chem. 38, 4739-4759 (1995).

2. M.F.G. Stevens, K.S. Phillip, D.L. Rathbone, D.M. O'Shea, S.F. Queener, C.H. Schwalbe and P.A. Lambert, J. Med. Chem. 40, 1886-1893 (1997).

3. V. Cody, N. Galitsky, J.R. Luft, W. Pangborn, A. Gangjee, R. Devraj, S.F. Queener & R.L.

Blakley, Acta Cryst. D53, 638-649 (1997).