Figure 3.

Systematic study with additional H₂O added to the reaction media. Standard conditions with peptide 2: 14 (1 equiv), 2 (10 mol %), 4-dimethylaminopyridine (10 mol %), H₂O₂ (30 wt %; 2.0 equiv), N,N′-diisopropylcarbodiimide (3.0 equiv total; 1 equiv @ 0 h, 4 h, 8 h), chloroform (0.1 M wrt 14), water (n + 15 equiv starting at 30 equiv), 4 °C, mixing @ 30 rpm, 24 h. Conversion and selectivity were determined by uncalibrated HPLC integrations of the crude reaction media (see Supporting Information for details).