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. 2000 Mar 9;43(5):829-42.
doi: 10.1021/jm990249v.

Synthesis, biological activity, and molecular modeling of ribose-modified deoxyadenosine bisphosphate analogues as P2Y(1) receptor ligands

Affiliations

Synthesis, biological activity, and molecular modeling of ribose-modified deoxyadenosine bisphosphate analogues as P2Y(1) receptor ligands

E Nandanan et al. J Med Chem. .

Abstract

The structure-activity relationships of adenosine-3', 5'-bisphosphates as P2Y(1) receptor antagonists have been explored, revealing the potency-enhancing effects of the N(6)-methyl group and the ability to substitute the ribose moiety (Nandanan et al. J. Med. Chem. 1999, 42, 1625-1638). We have introduced constrained carbocyclic rings (to explore the role of sugar puckering), non-glycosyl bonds to the adenine moiety, and a phosphate group shift. The biological activity of each analogue at P2Y(1) receptors was characterized by measuring its capacity to stimulate phospholipase C in turkey erythrocyte membranes (agonist effect) and to inhibit its stimulation elicited by 30 nM 2-methylthioadenosine-5'-diphosphate (antagonist effect). Addition of the N(6)-methyl group in several cases converted pure agonists to antagonists. A carbocyclic N(6)-methyl-2'-deoxyadenosine bisphosphate analogue was a pure P2Y(1) receptor antagonist and equipotent to the ribose analogue (MRS 2179). In the series of ring-constrained methanocarba derivatives where a fused cyclopropane moiety constrained the pseudosugar ring of the nucleoside to either a Northern (N) or Southern (S) conformation, as defined in the pseudorotational cycle, the 6-NH(2) (N)-analogue was a pure agonist of EC(50) 155 nM and 86-fold more potent than the corresponding (S)-isomer. The 2-chloro-N(6)-methyl-(N)-methanocarba analogue was an antagonist of IC(50) 51.6 nM. Thus, the ribose ring (N)-conformation appeared to be favored in recognition at P2Y(1) receptors. A cyclobutyl analogue was an antagonist with IC(50) of 805 nM, while morpholine ring-containing analogues were nearly inactive. Anhydrohexitol ring-modified bisphosphate derivatives displayed micromolar potency as agonists (6-NH(2)) or antagonists (N(6)-methyl). A molecular model of the energy-minimized structures of the potent antagonists suggested that the two phosphate groups may occupy common regions. The (N)- and (S)-methanocarba agonist analogues were docked into the putative binding site of the previously reported P2Y(1) receptor model.

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Figures

Figure 1.
Figure 1.
Structures of ribose-modified nucleotide analogues synthesized as ligands for the P2Y1 receptor. The corresponding ammonium salts were synthesized and tested for biological activity. Rigid compounds 4 and 5 are in the 2E (N) and 3E (S) conformations, respectively, as defined by the pseudorotational cycle. The anti-conformation (not shown) of 4 is favored.
Figure 2.
Figure 2.
Effects of deoxyadenosine bisphosphate derivatives on P2Y1 receptor-activated phospholipase C activity in turkey erythrocyte membranes: concentration-dependent stimulation of inositol phosphate formation by 2-MeSADP (□), compound 4a (▽), and compound 5 (○) and its inhibition in the presence of 30 nM 2-MeSADP by compound 4c (▲) and compound 5 (●). Membranes from [3H]inositol-labeled erythrocytes were incubated for 5 min at 30 °C in the presence of the indicated concentrations of 2-MeSADP or of test compound, either alone or in combination with 30 nM 2-MeSADP. The data shown are typical curves for at least three experiments carried out in duplicate using different membrane preparations.
Figure 3.
Figure 3.
(A) Side view of the 4a/P2Y1 receptor complex model. The side chains of the important residues in proximity to the docked 4a molecule are highlighted and labeled. Residues in proximity (≤5 Å) to the docked 4a molecule: Arg128(TM3), Tyr136(TM3), His277(TM6), Lys280(TM6), Gln307(TM7), Arg310(TM7), and Ser314(TM7). (B) Alignments generated by “Fit Atoms” analysis between 4a (green) and 5 (red).
Figure 4.
Figure 4.
(A) Superposition of docked P2Y1 antagonist structures, all of which contain an N6-Me group. The transmembrane helical bundle is not highlighted, but it conserves the same arrangement shown in Figure 3A: red = 1a; magenta = 4b; yellow = 6; blue = 7c. (B) Alignment of 4b (magenta) generated by “Fit Atoms” analysis using 1a (red) as reference structure.
Scheme 1.
Scheme 1.
Synthesis of N6-Methyl-2′-deoxyaristeromcyin Derivativesa a Reagents: (a) (1) MeI, DMF, (2) MH4OH, 90 °C; (b) DCTIDS/imidazole, DMF; (c) PhOCSCl/DMAP, CH3CN; (d) n-Bu3SnH/AIBN, toluene; (e) n-Bu4NF, THF; (f) LDA/TBPP; (g) (1) H2/Pd–C, (2) NH4HCO3.
Scheme 2.
Scheme 2.
Synthesis of N6-Methyl-(N)-methanocarbaadenosine-3′,5′-bisphosphatea a Reagents: (a) (1) MeI, DMF, (2) NH4OH, 90 °C; (b) LDA/TBPP/THF; (c) (1) H2/Pd–C, (2) NH4HCO3.
Scheme 3.
Scheme 3.
Synthesis of 2-Chloro-N6-methyl-(N)-methanocarbaadenosine-3′,5′-bisphosphatea a Reagents: (a) DEAD, Ph3P, THF; (b) MeNH2; (c) BCl3; (d) (1) LDA/TBPP, (2) BCl3.
Scheme 4.
Scheme 4.
Synthesis of a 9-Cyclobutyladenine Bisphosphate Derivativea a Reagents: (a) KOt-BU, heat; (b) HCC–COOEt, CH2Cl2, 50 °C; (c) DBU, DMF, rt; (d) LiAlH4, THF, 0 °C; (e) acetone, HCl, rt, NaBH4, MeOH, 0 °C; (f) POCl3, Proton Sponge, (CH3O)3PO, 0 °C; (g) NH4HCO3.
Scheme 5.
Scheme 5.
Synthesis of an 9-Anhydrohexitol Adenine Bisphosphate Derivativea a Reagents: (a) (1) MeI, DMF, (2) NH4OH, 90 °C; (b) POCl3, (MeO)3PO, Proton Sponge; (c) LDA/TBPP, THF; (d) (1) H2/Pd–C, (2) NH4HCO3.
Scheme 6.
Scheme 6.
Synthesis of an 9-Anhydrohexitol 2-Chloro-N6-methyladenine Bisphosphate Nucleoside Intermediatea a Reagents: (a) LiH, DMF; (b) 80% acetic acid, 60 °C.
Scheme 7.
Scheme 7.
Synthesis of Phosphonate Derivatives of Adeninylmorpholinea a Reagents: (a) NaIO4, H2O; (b) NH2(CH2)2PO3H2; (c) NABH3CN; (d) NH4HCO3.

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