Table 1.
entry | L | reaction time of step a (min.) | stoichimotetry of NaCN (equiv.) | yield (%)c |
---|---|---|---|---|
1 | L1 | 10 | 1 | 34d |
2 | L1 | 10 | 0.2 | 46 |
3 | L1 | 10 | 0.1 | 61 |
4e | L1 | 10 | 1 | 31 |
5 | L1 | 30 | 1 | 33 |
6f | L1 | 10 | 1 | 31 |
7 | L2 | 10 | 1 | 64 |
8 | L3 | 10 | 1 | 13 |
Reaction conditions: 1 (20 nmol), Pd complex (20 nmol), DMSO (200 μL), r.t., 10–30 min.; NaCN (aq.) in 10 μL H2O, 5 min.
AcNH-FLGKGVGCAF-CO2H.
Determined by integration of HPLC peak area with calibration.
Average of three runs.
Results with 1.5 equivalent of Pd complex.
Result with 0.1 M Tris buffer in DMSO/H2O (9:1) in place of DMSO.