Ammonia → HCID 88320517, compound

Participants

Reaction Steps

Ammonia gas was passed through a solution of the product of Example 9 (0.644 g) in dry methanol (50 ml) at -15° C. until saturated. The reaction flask was sealed with a rubber septum and allowed to stand at room temperature for 48 hours, then solvents were evaporated at reduced pressure. The residue was dissolved in acetonitrile (1 ml) and 2N aqueous hydrochloric acid (2 ml), and the solution freeze dried. The residue was boiled with ethyl acetate, allowed to cool, and the title compound collected by filtration as a colourless solid, mp 146°-148° C. Analysis Calcd. for C22H22F6N2 O2.HCl.H2O: C, 51.32; H, 4.89; N, 5.44; Found: C, 51.28; H, 4.73; N, 5.84%. MS (Cl+) 461 (M+H)+.

Provenance & Evidence