Reaktion #216068

Reaktionsgleichung

Val

Ile

Thr

Trp

Gly

→

Glycyl-glycyl-isoleucyl-tryptophyl-threonyl-tryptophyl-valine

Reaktionsbedingungen

Vorschrift

655 mg of the peptide-resin was treated with 1 mL of anisole and 10 mL of HF for one hour at 0° to 4° C. The HF was removed by nitrogen stream and the resultant solids were triturated with diethyl ether (30 mL). The solids were collected by filtration, washed with diethyl ether (3 ×10 mL) and then extracted with 70% acetic acid (3×10 mL). The extracts were combined and lyophilized to yield 128 mg of crude peptide. 84 mg of the crude peptide had the Trp residues deformylated by dissolution in 2% piperidine (10 mL) and stirring for 2 hours at room temperature. This solution was injected over three runs onto a Vydac 22×250 mm C18 10 μm particle sized 300 Angstrom pore packed column. Elution with a gradient of 30% to 50% B over 30 minutes at a flow rate of 10 mL/min was carried out (Solvent A= 0.1% TFA; Solvent B=0.1% TFA in 80% Ethanol/Water). Fractions were collected and the appropriate ones pooled to give 53 mg of white solid. Amino Acid Analysis: Gly 2.00 (2.00) , Ile 0.92 (1.00) , Thr 0.90 (1.00), Val 1.00 (1.00), Trp 1.79 (2.00), 61% peptide FAB/MS: MH+=818 (MW=817)

Quelle