Yields and purities of the 4 sequences synthesized under microwave irradiation using different deprotection reagents64.
Peptidea/base | Crude yield (%) | Purity (%) | Purified yield (%) | ||||||
---|---|---|---|---|---|---|---|---|---|
4-Me-piperidine | Piperidine | Piperazine | 4-Me-piperidine | Piperidine | Piperazine | 4-Me-piperidine | Piperidine | Piperazine | |
FISEAIIHVLHSR | 73.2 | 72.0 | 53.6 | 47.6 | 43.6 | 57.7 | 34.9 | 31.3 | 31.0 |
TLEEFSAKL | 99.1 | 98.4 | 99.4 | 65.1 | 83.0 | 74.8 | 64.5 | 81.7 | 74.3 |
KKWRWWLKALAKK | 93.6 | 81.6 | 74.7 | 50.4 | 59.1 | 55.6 | 44.4 | 48.2 | 41.5 |
VAPIAKYLATALAKW-ALKQGFAKLKS | 68.5 | 79.3 | 68.2 | 20.6 | 29.0 | 21.4 | 14.1 | 23.8 | 14.6 |
Coupling: 0.125 M concentration in DMF with DIC/Oxyma Pure, Rink Amide aminomethyl PS resin on a Liberty Blue™ (90 °C, 30 W, 110 s). Fmoc-removal: 20% 4-Me-piperidine (v/v) in DMF, or 20% piperidine in DMF (v/v), or 10% piperazine in 9 : 1 DMF/EtOH (w/v) on a Liberty Blue™ (90 °C, 30 W, 50 s). Prior to analysis peptides were cleaved from the resin and deprotected, precipitated with cold DEE, centrifuged, washed with cold DEE five times, dried, dissolved in water, lyophilized and analysed.