反应详情

5 mL of DMF and 400 μL of DIEA was added to 200 mg (0.63 mmol) HPMPC to produce a HPMPC-DIEA salt. Solvent was removed under vacuo and HPMPC-DIEA salt was carefully dried. 1.5 times excess of desired dipeptide from the general procedure described above was added to the dry HPMPC-DIEA salt, as well as 7 mL dry DMF and 400 μL DIEA. The mixture was heated for 1 h at 40° C. before 660 mg (1.3 mmol) PyBOP was added. Reaction was monitored by 31P NMR, and additional portions of PyBOP were added until the reaction was completed. Solvent was removed under vacuo, and purified by silica gel column chromatography [Solvent system: (CH2Cl2), (CH2Cl2: acetone, 2:1), (CH2Cl2: acetone: MeOH, 20:10:3)].