Picolinic acid → HCID 9951363, compound

Participants

Reaction Steps

The compound of Example 1(c) (0.95 g, 5.8 mmol) was dissolved in DMF (10 mL) and was treated at 0° C. with picolinic acid (2.14 g, 17.4 mmol), Bop reagent (7.70 g, 17.4 mmol), HOBt (2.35 g, 17.4 mmol) and iPr2EtN (10.1 mL, 58.0 mmol). After 20 h at RT, the solvent was evaporated under high vacuum. The residue was dissolved in CHCl3 and washed with 1 N HCl. Removal of solvent under reduced pressure gave crude product which was purified by flash chromatography (silica gel, 40% EtOAc in hexane) to give 430 mg of the desired material. This material was further recrystallized from CHCl3:EtOAc:Hexane (3:1:1) to give 230 mg of pure material. MS (ES+) m/z 373 [M+H]+.

Provenance & Evidence