Supporting Information for J. Org. Chem., 1994, 59(19), , DOI: /jo00098a042 DUEHOLM i

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1 Supporting Information for J. Org. Chem., 1994, 59(19), , DOI: /jo00098a042 DUEHOLM i \ 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 machine-readable 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 1994 American Chemical Society

2 T-KLD 3503.fid DATE: Jan FILE: exp SOLVENT: DHSO OBSERVE Hi FREQUENCY HHz SPECTRAL WIDTH Hz ACQUISITION TIHE sec RELAXATION DELAY sec PULSE WIDTH 10.0 usee TEMPERATURE 25.0 deg. C. NO. REPETITIONS 16 DOUBLE PRECISION ACQUISITION DATA PROCESSING FT SIZE TOTAL ACQUISITION TIME i minutes BocNH o 12a X 0 2H J L_-J _j [ j j j i j- _j,,,,! i r 5 4 i i i i -i i - r r ppm I V i ST "

3 T-KLD 3504.fid DATE: Jan FILE: exp SOLVENT: DMSO OBSERVE C13 FREQUENCY HHr SPECTRAL WIDTH Hz ACQUISITION TIME sec RELAXATION DELAY sec PULSE WIDTH 10.0 usee. TEMPERATURE 25.0 deg. C. NO. REPETITIONS 1024 DECOUPLE Hi HIGH POWER 45 DECOUPLER CONTINUOUSLY ON WALTZ-16 MODULATED DOUBLE PRECISION ACQUISITION DATA PROCESSING LINE BROADENING 2.0 Hz FT SIZE TOTAL ACQUISITION TIME 37 minutes BocNH 12a N..C0 2H J (\ioino ooi'h{\j(n -HooioiNincocafv! midn-hoi-rttdwaj 010)0101(D(DNa3CG cncnnnnmmcuaj N U lo ID ~i i i i i i i r I ' ' i i i i ] i i i r JOU "T I I I I I I I I I I I I I I I I ] I I I I I I 1 I ppm &

4 C-KLO 3505.fid DATE: Jan FILE: exp SOLVENT: DHSO OBSERVE Hi FREQUENCY MHz SPECTRAL WIDTH Hz ACQUISITION TIHE sec RELAXATION DELAY sec PULSE WIDTH 10.0 usee TEMPERATURE 25.0 deg. C. NO. REPETITIONS 16 DOUBLF PRECISION ACQUISITION DATA PROCESSING FT SIZE TOTAL ACQUISITION TIMF. 1 minutes BocNH' NHCbz,N^ 12b,COoH I T j 1 I I I I I I ~j I I I 1 T 1 I I I I I I I I I I [ I I I I I ppm 1 i " i " ; l/0~~ ^

5 C-KLD 3506.fid DATE: Jan FILE: exp SOLVENT: DMSO OBSERVE C13 FREQUENCY HHz SPECTRAL WIDTH Hz ACQUISITION TIME sec RELAXATION DELAY sec PULSE HIDTH 10.0 usee TEMPERATURE 25.0 deg. C. NO. REPETITIONS 2000 DECOUPLE HI HIGH POWER 45 DECOUPLER CONTINUOUSLY ON HALTZ-16 MODULATED DOUBLE PRECISION ACQUISITION DATA PROCESSING LINE BROADENING 2.0 Hz FT SIZE TOTAL ACQUISITION TIME 73 minutes BocNH NHCbz 12b N.,COoH ffl (\1 o cd m m w cn m cn cn cn <* > 03 w oi cn W m IN FN DO cn w rv o in in in D) CO S cn co O 2 o ni r* cn OJ ^ T CT) w* k J. i i i i [ i i i r [ i i i i j i i i i i i i i i i i i i ] i i i i i r i i i j i i i i i i i i i [ i i i i i i i " j i i i i i i i i i ] i i i i i i ' i i i i i i i i i i r ppm _C

6 A-KLD fid DATE: dan FILE: exp SOLVENT: DMSO OBSERVE Hi FREQUENCY 399,952 MHz SPECTRAL WIDTH Hz ACQUISITION TIME sec RELAXATION DELAY sec PULSE WIDTH 10.0 usee TEMPERATURE 25.0 deg. C. NO. REPETITIONS IB DOUBLE PRECISION ACQUISITION DATA PROCESSING LINE BROADENING 0.2 Hz FT SIZE TOTAL ACQUISITION TIME 1 minutes NHCbz.N..C 0 2H BocNH ^ 12c Ia i 1 i i j i i r~ i i r i i i i i i i i i i I r _J L. B.7B T T T T T T T T T _J L ppm < Q i c j \, L h! in

7 A-KLD 3508.fid DATE: Jan FILE: exp SOLVENT: OHSQ OBSERVE CIS FREQUENCY MHz SPECTRAL WIDTH Hz ACQUISITION TIME sec RELAXATION DELAY sec PUL.SE WIDTH 10,0 usee TEMPERATURE 25.0 deg. C. NO. REPETITIONS 2422 DECOUPLE HI HIGH POWER 45 DECOUPLER CONTINUOUSLY ON WALTZ-16 MODULATED DOUBLE PRECISION ACQUISITION DATA PROCESSING LINE BROADENING 2.0 Hz FT SIZE TOTAL ACQUISITION TIME 88 minutes in CN CD cn ^ CD M UJ v cn co o) QD N N (M cu cu ru ru lij \ NHCbz BocNH 12c N. ^C0 2H 03 oo cn M ID cu oi m cn oi cn m CD tvi cn tn in oi j in m m OJ -q- W T o CM" ~ in cu to 03 in oi O "T in T P ID CD u k k J 'Jr/M"».I wii im -».1,1.^.»"-fy J- f rtviyitiii'i VI MY ) *f > fynvagi-f^i' V.N '--. yi'f,u jtuhl/ Vtui.II r T i i i i i i r t [ i i i i ] i i i r j r THT-T I r ~i i i i i i i i i [ i i i i i i i i! j i i i i r PP cn / "5 v-

8 G-KLD 3509.fid DATE: Jan FILE: exp SOLVENT: DMSO OBSERVE Hi FREGUENCY MHz SPECTRAL WIDTH Hz ACQUISITION TIME sec RELAXATION DELAY sec PULSE WIDTH 10.0 usee TEMPERATURE 25.0 deg. C. NO. REPETITIONS 16 DOUBLE PRECISION ACQUISITION DATA PROCESSING LINE BROADENING 0.2 Hz FT SIZE TOTAL ACQUISITION TIME 1 minutes O ' BocNH' Ph 12d,c o 2h i j [ I j I I 1 T I I I 1 ] i I I I

9 G-KLD 3510.fid DATE: Jan FILE: exp SOLVENT: DHSO OBSERVE C13 FREQUENCY MHz SPECTRAL HIDTH Hz ACQUISITION TIME sec RELAXATION DELAY ec PULSE HIDTH 10.0 usee TEHPERATURE 25.0 deg. C. NO. REPETITIONS 1133 DECOUPLE HI HIGH POWER 45 DECOUPLER CONTINUOUSLY ON WALTZ-16 HODULATED DOUBLE PRECISION ACQUISITION DATA PROCESSING LINE BROADENING 2.0 Hz FT SIZE TOTAL ACQUISITION TIME 41 minutes H o N N BocNH N C02H in in m CO ID c n c n o i m cn ro CU CD CO CD 00 fo to cn cn cn on cn cn to ID i i j j r~i ] f 1 j > i i i i i i m p n i i \ i m i ] i i i i p i r n r~ I m r~ \ i r n r~] i i i i I i i i i j i i i r~j r i i r y ppm 3 o a

10 V J! 1 2U0 na (3rik) I 1 _ t i m 1 r I LTi H-GTA GAT CAC T-Lys-NH 2 D I 1 1 _ IT. 1 1 o- 1,^-! t t i i i i i i i i -i r rr, «i J ' '. i..., i. i i U (mi n 5!

11 LA_ i l) i la uu) H-GTA GAT CAC T-Lys-NH 2 ^ cn_ - cn D < \n cs CN : w o <r> 44. < i 1 ' ' ' r } 0 20 "I 1 r~ n, 1.. r- 30 (m i n) o 0k'

12 2liQ nn On in) CN H-AGT GAT CTA C-Lys-NH 2 3 < CM CM -» 1» 1 i 1 " I I 1 i, J. 2U 31) (mi H) Q 'i -fl

13 00. H-TGT ACG TCA CAA CTA-NH, C N _

14 [ MASS SPECTRUM J Data Samp le Mode R. T. Scan# 165 PNR58; 22/6-92; MF-FRB [Pos (1,6) 6'pjfr 56 ~S/7 >? r/r B. P i MSZ = Int. = o C.&Jt ^ M ^ DI(Deg.C) : i H-GTA GAT CAC T-Lys-NH in -i-j w i LP a

15 * f MRSS SPECTRUM J Data Samp 1e Mode R. T. : 164 : PNR60; 22/6-92; : MF-FRB [Pos.J ; Sc an # : (1,7) 6~f/rr' B.P. ; M/Z = Int. = DI(Deg.C) : H-AGT GAT CTA C-Lys-NH (SI (T ' j

16 ?wa cj^. z. <^9C a(2 ) mss SPECTRUM 3 Data Samp le Mode R.T. Scan# B.P. 2S5JS SK4; 29/12-92; MF-FRB CPos.J (1,.3) M/Z = Int. = 3.32 DI(Deg.C) : H-TGT ACG TCA CAA CTA-NH, J B rlilillillifliiiliiidii>i111nnib ii ? h/2 2: o 1 I l/l -u U) r t ^ f* 7 <L * Vx