Boron Trichloride → HCID 76903418, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of the product from step 1 (460 mg, 0.64 mmol) in anhydrous CH2Cl2 (15 mL) at −78° C. was added BCl3 (5.0 mL, 1M in DCM, 5.0 mmol), and the reaction mixture was stirred at same temperature for 1 hr, at which time the reaction mixture was warmed up to 0° C. and stirred at same temperature for additional 1 hr. The reaction was quenched by addition of water (5 mL) at 0° C. After the phase separation, the product in aqueous phase was purified by reverse phase preparative HPLC [Phenomenex Luna, 5 μm, 30×75 mm, 5-100% AcCN:H2O (with 0.1% TFA)] and dried using lyophilization to afford the product (10 mg) as while solid. ESI-MS m/z 395 (MH)+.

Provenance & Evidence