反应详情

Z-Leu-OSu (LXIII) (10.8 gm), and the above TFA salt (LXIV) (17.8 gm) in DMF (200 mg) and Et3N (8.4 ml), were stirred at room temperature for 24 hours. The reaction mixture was evaporated in vacuo and the resulting peptide was partitioned between H2O and CHCl3. The dried (Na2SO4) organic layer was evaporated and crystallized from acetone-MeOH to afford 17.7 gm (80%) of pure LXV: m.p. 138°-140°C; [α]D22 -35.4 (c, 1.16, MeOH); Rf1 0.86 and Rf3 0.68, single spot with I2 reagent. Amino acid analysis gave Leu 1.1; Arg 0.9; Pro 1.0; Gly 1.0; NH3 0.9.

1. customThe reaction mixture was evaporated in vacuo
2. customthe resulting peptide was partitioned between H2O and CHCl3
3. dry with materialThe dried (Na2SO4) organic layer
4. customwas evaporated
5. customcrystallized from acetone-MeOH
6. customto afford 17.7 gm (80%) of pure LXV