反应详情

A stirred mixture of 3-6 (147 mg, 0.46 mmol), HOBT (94 mg, 0.61 mmol), 2-1 (154 mg, 0.46 mmol), NMM (100 μL, 0.91 mmol), and DMF (1.2 mL) at 0° C. was treated with EDC (118 mg, 0.61 mmol) followed by removal of the cooling bath. The reaction pH was adjusted to 8 by addition of more NMM. After 20 h the reaction mixture was concentrated and the residue purified by to a flash chromatography column (silica, 9/0.5/0.5 CH2Cl2 /CH3OH/AcOH) to give 3-7 as a yellow solid after azeotropic removal of residual AcOH with toluene. Rf 0.48 (silica, 9/0.5/0.5 CH2Cl2 /CH3OH/AcOH).

1. customfollowed by removal of the cooling bath
2. additionThe reaction pH was adjusted to 8 by addition of more NMM
3. concentrationAfter 20 h the reaction mixture was concentrated
4. customthe residue purified by to a flash chromatography column (silica, 9/0.5/0.5 CH2Cl2 /CH3OH/AcOH)