Dicyclohexylcarbodiimide → HCID 67248269, compound

Participants

Reaction Conditions

Reaction Steps

DCC (0.433 g; 2.1 mmol) was added with vigorous stirring to a solution of the compound of example 66d (0.53 g; 1.9 mmol) and 1-hydroxybenzotriazole (0.338 g; 2.47 mmol) in dry DMF (15 ml) at 0° C. After 10 min. piperazin-1-yl-acetic acid ethyl ester (0.43 g; 2.47 mmol) was added to the mixture It was stirred at 0° C. for 1 h and then kept in the freezer over night. The DCU was filtered off and the filtrate was washed with 1N aqueous NaHCO3, water, 1N aqueous HCl, brine, dried (Na2SO4), concentrated and purified using flash chromatography (silica gel, 5% MeOH in chloroform) to obtain the title compound. Yield, 0.64 g (77%); mp, 189-90° C.; MS (ESI+): 450 (M++Na), analysis: C21H25N5O5 requires C, 59.01; H, 5.90; N, 16.38; found: C, 58.80; H, 5.93; N, 15.80%.

Provenance & Evidence