Pyridine → HCID 70663719, compound

Participants

Reaction Conditions

Reaction Steps

The compound of step 2 (0.576 g, 1.72 mmol) was dissolved in DCM (8 ml) under argon and cooled at 0° C. Pyridine (0.14 ml, 1.72 mmol) and triphosgene (0.509 g, 1.72 mmol) were added and the mixture was stirred at room temperature for 2 h. The mixture was then added dropwise to a solution of 1-tert-butoxycarbonyl-piperazine (1.28 g, 6.85 mmol) and triethylamine (0.86 ml, 6.85 mmol) in DCM (8 ml) cooled to 0° C. The mixture stirred at room temperature overnight, then diluted with 1 N hydrochloric acid and extracted with DCM. The combined organic phases were washed with a saturated sodium hydrogencarbonate solution and twice with a saturated sodium chloride solution, were dried over sodium sulfate, filtered and evaporated to dryness. The residue was purified by silica gel chromatography (cyclohexane/EA, 100:0, then 75:25) to give 0.895 g of the title compound as an off-white powder.

Provenance & Evidence