m-Chloroperbenzoic acid → HCID 14013758, compound

Participants

Reaction Steps

To a 0° C. solution of 4.8 g (0.012 mol) of product of Example 33 in 30 ml of CH2C2 was added 4.08 g (0.024 mol) of MCPBA. The reaction was monitored by TLC. The reaction mixture was filtered, washed with NaHCO3, dried (MgSO4) and concentrated in vacuo to give 4.56 g of solid which was purified by HPLC using 8% ehthyl acetate/cyclohexane to elute the first fraction (1.52 g) followed by 15% ethyl acetate cyclohexane to elute 1.46 g of the desired product. Recrystallization of the 1.46 g solid in hot hexane afforded 0.88 g (17.4%) of product as a white solid; mp 87°-88.5° C.

Provenance & Evidence