Trifluoroacetic acid → HCID 12016525, compound

Participants

Reaction Steps

A solution of Example 1D (3.0 g, 6.5 mmol) in dichloromethane (30 mL) at 0° C. was treated, over a period of 10 minutes, with trifluoroacetic acid (7.5 mL, 97 mmol). The reaction mixture was allowed to warm to room temperature, stirred for 24 hours, and concentrated. The concentrate was dissolved in dichloromethane (300 mL) and the solution was washed sequentially with saturated NaHCO3, water, and brine, dried (MgSO4), filtered, and concentrated. The concentrate was dissolved in methanol (120 mL), treated with L-tartaric acid (1.0 equivalent based on recovered material), stirred for 18 hours at room temperature, and concentrated. The concentrate was dissolved in water (25 mL) and lyophilized to afford the desired product in 83% yield.

Provenance & Evidence