Hydrogen Bromide → HCID 131722982, compound

Participants

Reaction Steps

To a suspension of the product from Example 170 (1.0 g, 2.0 mmol) in ethanol (16.6 mL) was added hydrobromic acid solution (30 wt % in acetic acid, 2.0 mL, 10.0 mmol) at 20° C. while stirring. The yellow slurry was stirred at r.t. for 3 h, and DSC analysis on a filtered wet sample showed a melt endotherm at ˜260° C. The slurry was filtered, and the filter cake was washed with 40 mL of ethanol and dried at 45° C. vacuum over for 24 h. The product was obtained as a pale yellow solid (1.1 g, 92% yield) with a HPLC purity of 99%; mp 244-248° C.; Anal. Calcd for C23H22ClN9O2.HBr: C, 48.22; H, 4.05; N, 22.01; Cl, 6.19; Br, 13.95. Found: C, 48.02; H, 3.98; N, 21.87; Cl, 6.13; Br, 13.83.

Provenance & Evidence