Triethylamine → HCID 178467737, compound

Participants

Reaction Steps

A solution of the title compound of Example 5 (540.3 mg), 3-butyn-2-ol (0.13 mL), PdCl2 (PPh3)2 (21.1 mg), and 0.75 mL Et3N in 3 mL DMF is heated at 90° C. for 1 hr. The reaction mixture is cooled to room temperature and partitioned between EtOAc and H2O. The aqueous layer is washed with EtOAc (3×). The combined organic layers are dried over Na2SO4 and condensed to obtain a brown residue. The residue is diluted with MeOH, adsorbed onto silica, and chromatographed eluting with 2.5 % MeOH in CH2Cl2. Fractions homogenous by TLC are combined, condensed and recrystallized from EtOAc/hexanes to yield 0.207 g of the desired product as a creme-colored solid.

Provenance & Evidence