J. Am. Chem. Soc., 1997, 119(5), , DOI: /ja962780a
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1 J. Am. Chem. Soc., 1997, 119(5), , DOI: /ja962780a Terms & Conditions Electronic Supporting Information files are available without a subscription to ACS Web Editions. The American Chemical Society holds a copyright ownership interest in any copyrightable Supporting Information. Files available from the ACS website may be downloaded for personal use only. Users are not otherwise permitted to reproduce, republish, redistribute, or sell any Supporting Information from the ACS website, either in whole or in part, in either machinereadable form or any other form without permission from the American Chemical Society. For permission to reproduce, republish and redistribute this material, requesters must process their own requests via the RightsLink permission system. Information about how to use the RightsLink permission system can be found at Copyright 1997 American Chemical Society
2 Pseudo-Prolines (PPro) as a Molecular inge: Reversible Induction of Cis Amide Bonds into Peptide Backbones. Pascal Dumy, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten Wohr and Manfred Mutter. Contribution from the Institute of Organic Chemistry, University of Lausanne, BC-Dorigny, C- 1015, Lausanne, Switzerland. Spectra were recorded at 400 MI-Lz using a Bruker ARX spectrometer at 300 K. Samples of around 25 mg were dissolved in ml of DMSOd 6. Chemical shifts were calibrated on the solvent isotopic impurity (2.49 ppm at 300 K). 2D experiments were typically acquired using 2K x 512 matrices over a 4000 z sweep width in both dimensions. Quadrature detection in the indirect dimension was achieved by using the TPPI procedurel. Scalar connectivities were recovered from 2D double quantum filtration (DQF) COSY experiments 2. Dipolar connectivities were obtained either through the conventional NOESY sequence 3 or the ROESY sequence 4 with mixing times from 150 to 200 ms. A randomization of the mixing length (± 5%) was introduced in the NOESY experiments in order to minimize coherence transfer. The spin lock mixing interval of the ROESY sequence was applied by coherent CW irradiation at yb 2 /2xr = 2 Kz. Experimental data processing was performed using the Felix software package 5. The standard sinebell squared routine was employed for apodization with a shift range of and zero filling in both dimensions before 2D transformations were applied to end up with square matrices of 2K x 2K real point data. Complete proton resonance assignments were made using (DQF) COSY experiments, MQC was used to assign unambiguously the carbon resonances. J coupling constant were directly measured from highresolution ' -ID spectra (±0.1z) or simulated for complex or overlapped systems. Prochiral assignments for the 'Pro P and Me protons were achieved, in some cases, on the basis of relative interproton ROE intensities and J coupling constant values. 1 Drobny, G.; Pines, A., Sinton, S.; Wertekamp, D.; Wemmer, D. Faraday Div. Chem. Soc. Symp., 1979, 13, Piantini, V.; Sorensen, 0. W.; Ernst, R. R. J Am. Chem. Soc,. 1982, 104, Jeener, J.; Meier, B..; Bachmann, P.; Ernst, R. R. J Chem. Phys., 1979, 71, Bothner-By, A. A.; Stephen, R. R-L.; Lee, J., Warren, C. D.; Jeanloz, R. W., J Am. Chem. Soc. 1984, 106, Biosym Technologies Inc., San Diego. Pseudo-Prolines (YPro) as a Molecular inge: Reversible Induction of Cis Amide Bonds into Peptide Backbones. Pascal Dumy, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten W6hr and Manfred Mutter.
3 Ac-Ala-Ser(MeMepro)N-Me (1) pros 0 Table 1. 1 NMR spectral parameters of compounds 1. N ('JN-a) a 3 a-p) ( 2 jp-p) 2-Me Ala (7.0) Ser(Yue~mepro) (6. lpro-r) 4.17/ Pro-R( 8.8) 1.52/ pro-s NMe 8.176(4.5) Ac Table C NMR spectral parameters of compounds 1. O p 2-C 2-Me CO Ala ser pro-s/ Ac 21.8 Me 25.8 Pseudo-Prolines (TPro) as a Molecular inge: Reversible Induction of Cis Amide Bonds into Peptide Backbones. Pascal Dumy, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten Wohr and Manfred Mutter.
4 Ac-Ala-Thr(TMeMepro)N-Me (2) N Me 0 NMe Table 3. 1 NMR spectral parameters of compounds 2. N ( 3 JN-) c a-) ( 2 p-p-i) PMe 2-Me Ala (6.6) - Thr(Y M e* M epro) (5.7) /1.50os NMe (3.6) Ac Table NMR spectral parameters of compounds 2. OX 0 PMe C(2) 2-C CO Ala Thr(" m ''"pro) pro-s/ Ac Me 25.8 Pseudo-Prolines ('VPro) as a Molecular linge: Reversible Induction of Cis Anide Bonds into Peptide Backbones. Pascal Dumy, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten W6hr and Manfred Mutter.
5 Ac-Ala-Cys(TMeMepro)N-Me (3) pros Me N. 0 Table 5. 1 NMR spectral parameters of compounds 3. N ('JN-a) C3 ajo-o) 2 P-P) 2-Me Ala 8.21(6.9) Cys(FueM'pro) ( 6.4ro-R) pro-r/ (11.8) / ro-s NMe 8.176(4.7) 2.85 Ac Table 6. 1 NMR spectral parameters of compounds 3. a. 0 2-Me CO Ala Cys(YMeMepro) pro-s/ Ac Me 25.3 Pseudo-Prolines (TPro) as a Molecular inge: Reversible Induction of Cis Anide Bonds into Peptide Backbones. Pascal Dumy, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten W6hr and Manfred Mutter.
6 Ac-Ala-Ser(T,pro)N-Me (4) 0) pros N NMe Table 7. 1 NMR spectral parameters of compounds 4. N ( 3 JNl-ly) cc P ( 2 JfW.P{1) y 2- Ala 8.219(5.8) (6.90) - Ser(pro) / /4.96(3) Ser(Ypro) / Cis(28%) NMe 7.78(4.5) 2.57 NMe Ac 1.81 Table C NMR spectral parameters of compounds 4. cx y 2-C CO Ala Ser(YPpro) Ser(PIlpro) Cis Ac Me 25.4(25.7) Pseudo-Prolines (TPro) as a Molecular inge: Reversible Induction of Cis Amide Bonds into Peptide Backbones. Pascal Duny, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten W~hr and Manfred Mutter.
7 Ac-Ala-Pro-N-Me (5) 0 pros N 0 NMe Table 9. 1 NMR spectral parameters of compounds 5. N ( 3 JN-o) X ( 3 Ja.-O) (2j P-P) y 5 Ala trans(82%) 8.05(7.5) (6.9) - - Pro trans - 4.2(3.8/8.4) P-'/ pro-r 1.88/ pro-r/ pro-s Ala Cis (18%) 7.99(7.3) (6.8) - - Pro Cis - 4.3(3.4/7.3) / /3.36 Me trans (4.7) Me cis (4.7) Ac 1.79 Table C NMR spectral parameters of compounds 5. a p y 6 CO Ala trans Pro trans Ala Cis Pro cis Ac Me 25.4 Me 25.7 Pseudo-Prolines ('PPro) as a Molecular inge: Reversible Induction of Cis Amide Bonds into Peptide Backbones. Pascal Dumy, Michael Keller, Declan E. Ryan. Barbara Rohwedder, Torsten Wahr and Manfred Mutter.
8 Succinyl-Val-Ser( pro)-phe-pna (7) Table NMR spectral parameters of compound 7 N('JN-a) cx (Jcc-P) 3 ( 2 Jp-a) Val 8.202(8.2) Ser('F pro) (7.3/ 5..0) 4.174pro-R (8.7) Phe Succinyl (4-NO 2 )-Ph (7.1) (5.4, 8.4) 8.2 (9.3) meta (13.8,) 7.79 ortho 0.865(6.6) /0.855(6.6) (3.7) 4.95 Pseudo-Prolines (TPPro) as a Molecular inge: Reversible Induction of Cis Anide Bonds into Peptide Backbones. Pascal Duny, Michael Keller. Declan E. Ryan, Barbara Rohwedder, Torsten W3hr and Manfred Mutter.
9 Succinyl-Val-Ser(Tm',mepro)-Phe-pNA (8) Table NMR spectral parameters of compound 8. N( JN-a) c. (3 Ja-P) P( 2JP-a) y 2-Me Ser(' MeMepro) (6.5,/1.9) pro-r (9.1) Phe 8.46 (7.7) Val 7.84 (8) 4.27 (6.2) (6.8) 0.88 (6.8) Succinyl 2.45 (4-NO2)-Ph (9.3) meta 7.77 ortho Pseudo-Prolines ('TPro) as a Molecular linge: Reversible Induction of Cis Anide Bonds Into Peptide Backbones. Pascal Duny, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten W6hr and Manfred Mutter.
10 Succinyl-Val-Ser( Y(2-R),PM PrO)-Phe-pNA (9) Table NMR spectral parameters of compound 9 N( 3 JN-x) a ('Jcx-P) Val trans (90%) (8.5) (8.8) (2j J-P) (6.6) / (6.7) Ser(W PMPpro) trans 4.65 (7.4/5.6) 4.122pro-R/ (8.9) Val Cis (10%) (6.5) Ser( PMP pro) cis / Phe trans 8.52 (7.2) 4.71 (5.9/8.4) / 3.01 (14) Phe cis (7.23) Succinyl 2.4 PMP 3.728(OMe) 6.98 (8.7) meta 7.71 ortho NO2Ph trans (9.3) meta 7.8 ortho Table C NMR spectral parameters of compound 9. a. P y 2-C Val trans /19 - Ser(PW, pro) trans Phe Suc PMP 55 (OMe) 113 meta 130 ortho (4-NO2)-Ph meta ortho Pseudo-Prolines ('PPro) as a Molecular inge: Reversible Induction of Cis Anide Bonds Into Peptide Backbones. Pascal Durny, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten Wahr and Manfred Mutter.
11 Succinyl-Val-Ser(W(2-S)PMPpro)-Phe-pNA (major) (10) Table NMR spectral parameters of compound 10. N ( 3 JN-a) a ( 3 Jc-O) 0(2JP-P) Val trans (50%) 7.53(8.9) 4.00 (8.3) 2.00 Ser(YPP trans ", pro) Val cis (50%) Ser(TPM., pro) cis Phe trans Phe cis Succinyl cis Succinyl trans PMP trans PMP cis (4-NO2)Ph trans (4-NO2)Ph cis (7.2/3.1) 7.65 (9.1) 4.44 (4.7/8.9) (6.3,/1.9) (7.2) (5.7/8.7) 8.89 (7.5) (7.0 /7.2) (OMe) 6.9(8.5) meta 3.74 (OMe) 6.88(8.5) meta (9.3) meta (9.3) meta pror (9.3) pro R 4.02 (8.9) (13.8), (14), ortho 7.29 ortho 7.8 ortho 7.77 ortho y 0.79(6.6)0.7 44(6.8) 0.82 (6.6), 0.69 (6.8) Table C NMR spectral parameters of compound 10. Val trans a y / C Ser( PMP, pro) trans Phe trans Val cis /16.6 Ser(Tp'l", pro) cis Phe cis Suc NO2PhN meta meta PMP 54.7 (OMe) meta ortho Pseudo-Prolines ('Pro) as a Molecular inge: Reversible Induction of Cis Anide Bonds into Peptide Backbones. Pascal Dumy, Michael Keller, Declan E. Ryan, Barbara Rohwedder, Torsten W6hr and Manfred Mutter.
12 L) - Y *, 111 Ac-Ala-Ser['P Mo 101 to 115 Kcal.morl am 116 to 130 Kcal.mor 131 to 145 Kcal.molpro]-NMe 180 Trans conformation E=20.1Kcal.mol' Cis conformation E=19.9 Kcal.mol' mm 101 to 115 Kcal.mol 116 to 130 Kcal.mol to 145 Kcal.mol
13 -~-~ j Trans conformation E=27.5 Kcal. mot' Ac-Ala-Pro-NMe 180 Cis conformation E=29.9 Kcal.mo' I Pt m 81 to 95 Kcal.mol) 96 to 110 Kcal.mol" Ill to 125 Kcal.mol m 83 to 97 Kcal.mol 98 to 112 Kcal.niol, 113 to 127 Kcal.mol"
14 II -~ Ii Ac-Ala-Ser[P MeMe pro]-nme Trans conformation E= Kcal.mor' Cis conformation E= Kcal.mot C) ac oo to 61 Kcal.mol - 62 to 76 Kcal.mol' 77 to 91 Kcal.mol to 46 Kcal.mol" - 47 to 61 Kcal.mol 62 to 76 Kcal.mol
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