Ring-Closing Metathesis Approaches for the Solid- Phase Synthesis of Cyclic Peptoids

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1 Supporting Information (SI) Ring-Closing Metathesis Approaches for the Solid- Phase Synthesis of Cyclic Peptoids Sharaf awaz Khan, Arim Kim, Robert. Grubbs, and Yong-Uk Kwon*, Department of Chemistry and ano Science, Ewha Womans University, Seoul 12-75, South Korea; The Arnold and Mabel Beckman Laboratory of Chemical Synthesis, Division of Chemistry and Chemical Engineering, California Institute of Technology, Pasadena, California 91125, USA. Table of contents General methods S2 Peptoid synthesis S2 General procedure for RCM of peptoids under microwave conditions S2 General procedure for RCM of peptoids at 4 o C S3 General TFA cleavage procedure and reverse-phase PLC S3 zonolysis of cyclic peptoid S3 Abbreviations S3 References S3 Table S1. MALDI-MS data of synthesized peptoids S4 Figure S1. Amines and RCM catalysts employed in this study S5 Table S2. RCM of peptoids (1-4) containing allylamines S5 Figure S2-S22. Schemes, PLC chromatograms and MALDI-TF spectra S6-S26 S1

2 General methods Chemical reagents were purchased from commercial sources and were used without further purification unless noted otherwise. Methylamine was used as 2 M solution in TF and glycine tert-butyl ester acetic acid was neutralized with aq. a 2 C 3 and extracted with DCM prior to use. Moisture sensitive reactions were performed under nitrogen or argon atmosphere. C 2 Cl 2 was dried over calcium hydride. Grubbs Catalyst 1st generation (G1), Grubbs catalyst 2nd generation (G2) and oveyda-grubbs Catalyst 2 nd Generation (G2) were purchased from Aldrich. Rink Amide AM resin LL (.4 mmol/g) and TentaGel MB RAM (.4 mmol/g) were purchased from ovabiochem. Reverse-phase PLC experiments were conducted through an ACE 5 C18-L (25 x 4.6mm) reverse phase column on a Shimadzu binary PLC system equipped with a UV-visible detector at 22 nm. The typical flow rate for analytical PLC was 1 ml/min. In all cases, a gradient elution of water/acetonitrile with.5% TFA was used. MALDI-TF MS was performed on a Voyager-DE STR biospectrometry workstation (Applied Biosystems) with α- hydroxy cinnamic acid as a matrix. The peptoids were synthesized in an incubator shaker (JEI TEC, model SI-6R) or in a microwave oven (Daewoo, model KR-B2R). The microwave reactions were performed at a power of 1 W for peptoid synthesis and at a power of 3 W for RCM reactions. Peptoid synthesis Peptoids were synthesized on Rink amide (1-5, 7-1, and 19-23) and TentaGel (24-29) resins by the conventional submonomer strategy. 1 Peptoid syntheses were performed in 25 ml standard glass peptide synthesis vessels. The resins were swelled in DMF at 25 o C for 1-2 h. Then DMF was drained, and the beads were incubated 2% piperidine in DMF for 1 h and washed thoroughly with DMF (8 x 3 ml). The beads were treated with 2 M bromoacetic acid ( ml) and 3.2 M DIC (1-1.5 ml) and irradiated in a microwave oven (1 W) for 3 x 12 sec with shaking for 3 sec after each pulse. The beads were thoroughly washed with DMF (8 x 3 ml) and then treated with primary amines (1-2 M, 2 ml) in DMF in a microwave oven (1 W) for 3 x 12 sec with shaking for 3 sec after each pulse. Both acylation and displacement were successively repeated to form the desired peptoid sequences. To prevent inactivation of RCM catalyst from free amines, the peptoids were capped with -anhydride (1 eq.) and triethylamine (1 ml) in DCM (5 ml) and the beads were shaken for 2 h before being washed with Me (8 x 3 ml) and DCM (8 x 3 ml), and left to dry under vacuum for 2 h before RCM. General procedure for RCM of peptoids under microwave conditions The beads (15 mg) containing linear peptoids were swelled in DCB (1 ml) in reaction vessel for 3 min. Then 2 mol% RCM catalysts were added and irradiated under microwave (3 W) for 4 x 3 sec (total 2 min) with shaking for 3 sec after each pulse. The resin was thoroughly washed with DCM (8 x 3 ml). S2

3 General procedure for RCM of peptoids at 4 o C The beads (15 mg) containing linear peptoids were charged in reaction flask and allowed to swell in anhydrous DCM (1 ml) for 3 min. Then 2 mol% RCM catalysts were added and refluxed at 4 o C under nitrogen atmosphere for 2 h. The resin was thoroughly washed with DCM (8 x 3 ml). General TFA cleavage procedure and reverse-phase PLC Peptoid-tethered resin was suspended in a cleavage cocktail (/5% 2 /3% TIS) for 1-2 h. After cleavage solution was removed by blowing 2 gas, 5% aq. acetonitrile containing.1% TFA was added and mixed uniformly. The mixture was filtered through.2 µm PTFE filter tip and the obtained solution was directly used for PLC and MALDI-TF analyses. Reverse-phase PLC experiments were conducted through a C18 reverse phase column on a Shimadzu binary PLC system by using a gradient elution of water/acetonitrile with.1% TFA. RCM products were produced as a mixture of E/Z isomers. zonolysis of cyclic peptoid The requisite cyclic peptoid was cleaved from resin by a cleavage cocktail, concentrated and dried. Then cyclic peptoid was dissolved in DCM and cooled to -78 o C. zone gas was purged through the cooled solution, which turned blue after a few minutes. Then ozone was bubbled further for 1 min. Dimethylsulfide was added to the reaction mixture which turned it into clear solution. The reaction mixture was warmed slowly to room temperature and the solvent was removed in vacuo. Abbreviations DMF:,-dimethylformamide, DCB: 1,2-dichlorobenzene, DCE: 1,2-dichloroethane, DCM: methylene chloride, TFA: trifluoroacetic acid, TIS: triisopropylsilane, DIC:, -diisopropylcarbodiimide, G1: Grubbs Catalyst 1 st generation [bis(tricyclohexylphosphine) benzylidine ruthenium(iv) chloride], G2: Grubbs catalyst 2 nd generation [1,3-bis-(2,4,6-trimethylphenyl)-2- (imidazolidinylidene)(dichlorophenylmethylene)(tricyclohexylphosphine) ruthenium], G2: oveyda- Grubbs Catalyst 2 nd Generation [(1,3-bis-(2,4,6-trimethylphenyl)-2-imidazolidinylidene)dichloro(oisopropoxyphenylmethylene)ruthenium], RCM: ring-closing metathesis, PLC: high-performance liquid chromatography, MALDI-TF: matrix-assisted laser desorption/ionization-time of flight. References 1. Zuckermann, R..; Kerr, J. M.; Kent, S. B..; Moos, W.. J. Am. Chem. Soc. 1992, 114, livos,. J.; Alluri, P. G.; Reddy, M. M.; Salony, D.; Kodadek, T. rg. Lett. 22, 4, S3

4 Table S1 MALDI-MS data of synthesized peptoids Entry Peptoid MS (calcd.) MS (obs.) [M+] + [M+a] + 1 3a b c a b c a a a a a a a a a a a a a a a a a 28a 29a S4

5 Figure S1. Amines and RCM catalysts employed in this study Methylamine Isobutylamine 2-Methoxyethylamine Furfurylamine Allylamine (ala) (leu) (mea) (ffa) (all) 2 3-Buten-1-amine (bte) ,4-diaminobutane (lys)* Glycine tert-butyl ester (asp)* Piperonylamine (pip) * lys and asp: protecting groups ( and tert-butyl) were removed with the treatment of at the cleavage step. Ring-closing metathesis catalysts PCy 3 Mes Mes Mes Mes Cl Cl Ru Ph PCy 3 Cl Cl Ru Ph PCy 3 Cl Cl Ru G1 G2 G2 Table S2. RCM of peptoids (1-4) containing allylamines R n 1: n = 2, all-leu-ffa-all 2: n = 3, all-leu-mea-ala-all 3: n = 4, all-leu-ffa-leu-mea-all 4: n = 6, all-mea-leu-ffa-ala-mea-leu-all Entry Peptoid Catalyst Solvent Temp. Time (h) Remarks 1 4-mer (1) G1 DCM o RCM 2 4-mer (1) G2 DCM o RCM 3 5-mer (2) G1 DCM o RCM 4 5-mer (2) G2 DCM o RCM 5 5-mer (2) G2 DCB o RCM 6 5-mer (2) G2 DCE o RCM 7 5-mer (2) G2 DCM MW 3 min o RCM 8 6-mer (3) G2 DCM o RCM 9 6-mer (3) G2 DCM 4 48 o RCM 1 6-mer (3) G2 DCB 8 24 o RCM 11 6-mer (3) G2 DCE 8 24 o RCM 12 6-mer (3) G2 DCB MW 2 min 1-2% 12 8-mer (4) G1 DCM o RCM 13 8-mer (4) G2 DCM o RCM 14 8-mer (4) G2 DCM MW 3 min o RCM 15 8-mer (4) G2 DCB MW 2 min 1-2% S5

6 1. G2, DCB 3W µwave, 2min 2 3 3a (after cleavage) 2 + 3b 2 Detector A:22nm 3 3c a + 3b 3c min Voyager Spec #1[BP = 67.4, 13743] E a b Voyager Spec #1[BP = 234.1, 12544] c Figure S2. RCM of peptoid 3 using G2 under microwave: PLC chromatogram and MALDI- TF spectra. S6

7 4 4a (after cleavage) 1. G2, DCB 3W µwave, 2min 2 4b Detector A:22nm 3 4c a + 4b 4c min Voyager Spec #1[BP = 87.8, 2374] b 4a Voyager Spec #1[BP = 193., 9274] c Figure S3. RCM of peptoid 4 using G2 under microwave: PLC chromatogram and MALDI- TF spectra. S7

8 2 5 5a 1. G2, DCB 3W mwave, 2min a 25 Detector A:22nm a Common impurity min 3 Detector A:22nm 25 2 Common impurity a min 1 Voyager Spec #1[BP = 75.4, 399] Voyager Spec #1[BP = 677.3, 3413] 3.E a Voyager Spec #1[BP = 234., 2388] E a Figure S4. RCM of peptoid 5 using G2 under microwave: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S8

9 G2, DCM 4 o C, 2h 7a 2 Detector A:22nm a Common impurity min Detector A:22nm 3 25 Common impurity min Voyager Spec #1[BP = 44.1, 659] a Voyager Spec #1[BP = 376.2, 359] E Figure S5. RCM of peptoid 7 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S9

10 8 1. G2, DCM 4 o C, 2h 2 8a 2 Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 475.1, 21631] E a Voyager Spec #1[BP = 447.4, 361] E Figure S6. RCM of peptoid 8 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S1

11 G2, DCM 4 o C, 2h 9a 2 13 Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 546.2, 12481] E a Voyager Spec #1[BP = 518.2, 19176] E Figure S7. RCM of peptoid 9 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S11

12 G2, DCM 4 o C, 2h 1a 3 Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 617.2, 2382] a Voyager Spec #1[BP = 589.4, 3437] Figure S8. RCM of peptoid 1 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S12

13 15 1. G2, DCM 4 o C, 4h 2 15a Detector A:22nm a min 25 Detector A:22nm min Voyager Spec #1[BP = 439.1, 21596] E a Voyager Spec #1[BP = 433.2, 362] Figure S9. RCM of peptoid 15 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S13

14 G2, DCM 16a 4 o C, 4h 2 Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 185.1, 15895] E a Voyager Spec #1[BP = 482.4, 271] E Figure S1. RCM of peptoid 16 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S14

15 G2, DCM 4 o C, 2h 19a 2 3 Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 514.2, 2592] a Voyager Spec #1[BP = 464.4, 7762] Figure S11. RCM of peptoid 19 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S15

16 G2, DCM 4 o C, 2h 2a 2 Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 627.5, 1799] E a Voyager Spec #1[BP = 577.6, 159] E Figure S12. RCM of peptoid 2 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S16

17 G2, DCM 4 o C, 2h 2 21a 2 Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 742., 53] a Voyager Spec #1[BP = 714.4, 2241] Figure S13. RCM of peptoid 21 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S17

18 G2, DCM 4 o C, 2h 22a Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 212., 585] a Voyager Spec #1[BP = 234., 997] Figure S14 RCM of peptoid 22 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S18

19 G2, DCM 4 o C, 2h 23a 34 3 Detector A:22nm 25 23a min Detector A:22nm min Voyager Spec #1[BP = 855.3, 1158] a Voyager Spec #1[BP = 827.6, 3944] Figure S15. RCM of peptoid 22 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S19

20 G2, DCM 4 o C, 2h 24a 2 25 Detector A:22nm a min 3 Detector A:22nm min Voyager Spec #1[BP = 527.3, 2153] a Voyager Spec #1[BP = 499.4, 189] Figure S16. RCM of peptoid 24 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S2

21 G2, DCM 4 o C, 4h 25a 2 Detector A:22nm a min Detector A:22nm min Voyager Spec #1[BP = 75.4, 1687] a 1.7E Voyager Spec #1[BP = 677.5, 877] Figure S17. RCM of peptoid 25 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S21

22 G2, DCM 4 o C, 2h 26a Detector A:22nm 37 26a min Detector A:22nm min Voyager Spec #1[BP = 75.4, 963] a Voyager Spec #1[BP = 234., 1372] Figure S18. RCM of peptoid 26 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S22

23 G2, DCM 4 o C, 2h 27a 2 Detector A:22nm a min 3 Detector A:22nm min Voyager Spec #1[BP = 818.6, 961] a Voyager Spec #1[BP = 79.6, 18326] E Figure S19. RCM of peptoid 27 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S23

24 G2, DCM 4 o C, 2h 28a Detector A:22nm 75 28a min Detector A:22nm min Voyager Spec #1[BP = 212., 585] a Voyager Spec #1[BP = 77.5, 5711] Figure S2. RCM of peptoid 28 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S24

25 29 1. G2, DCM 4 o C, 4h a 2 Detector A:22nm a min 25 Detector A:22nm min Voyager Spec #1[BP = 892.7, 831] a Voyager Spec #1[BP = 842.7, 1146] Figure S21. RCM of peptoid 29 using G2 at 4 o C: PLC chromatograms before RCM and after RCM, and MALDI-TF spectra. S25

26 2 1) 3, C 2 Cl 2, 1min, -78 o C 2) Me 2 S 2 C C (x1,) Detector A:22nm min (x1,) Detector A:22nm min Voyager Spec #1[BP = 714.4, 2241] Voyager Spec #1[BP = 746.2, 378] Figure S22. zonolysis of cyclic peptoid 32: PLC chromatograms before ozonolysis and after ozonolysis, and MALDI-TF spectra. S26

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