Triphenylphosphine → HCID 58664172, compound

Participants

Reaction Steps

A solution of 2-1a (0.21 g, 0.51 mmol) and triphenylphosphine (0.133 g, 0.51 mmol) in THF (10mL) was allowed to stir at rt overnight. The reaction was quenched with water (10 mL) and heated at 60° C. for 1 h. The product was extracted with EtOAc (2×30 mL) and washed with brine (30 mL), dried over MgSO4, filtered and concentrated. The remaining oil was dissolved in CH2CL2 (5 mL)I TFA (2 mL) and allowed to stir at rt overnight. The solvent was removed in vacuo. The remaining oil was dissolved in CH3CN (3 mL) and purified on a Gilson automated system affixed with a YMC J'sphere H80 30×100 mm column (eluting with 5-95% CH3CN +0.1% TFA in water +0.1% TFA over 20 min) to afford pure 2-3a.

Provenance & Evidence