反应详情

To a mixture of Boc-Leu-DTrp(COOMe)-OH (50 mg), H-DNle-OBzl.TsOH (46 mg), NMM (13 μl) and HOBT.H2O (16 mg) in dichloromethane (1 ml) was added EDCI.HCl (22 mg) under ice cooling. After being stirred at room temperature for 2 h, the mixture was diluted with dichloromethane, washed with water, 10% aq. citric acid, sat. aq. NaHCO3 and brine successively, dried over MgSO4 and evaporated in vacuo. The residue was purified by preparative TLC (Merck, Kieselgel 60 F254) with chloroform/methanol/acetic acid=100/10/1 for development to give Boc-Leu-DTrp(COOMe)-DNle-OBzl (67 mg).

1. washwashed with water, 10% aq. citric acid, sat. aq. NaHCO3 and brine successively
2. dry with materialdried over MgSO4
3. customevaporated in vacuo
4. customThe residue was purified by preparative TLC (Merck, Kieselgel 60 F254) with chloroform/methanol/acetic acid=100/10/1 for development