Hydrogen Bromide → HCID 86694432, compound

Participants

Reaction Steps

A suspension of the racemic product of Example 1 (1.77 g, 4.69 mmol) in 33% HBr in acetic acid (30 mL) was stirred at ambient temperature for 2 hours. The reaction mixture was concentrated to a crude solid/liquid mixture. Ethanol (35 mL) was added, and the resulting suspension was stirred at ambient temperature. The solids were filtered, rinsing the filter cake with ethanol. The filtered solids were dried on the high vacuum until constant weight was achieved to afford the desired product (HBr salt) as a grey solid. LRMS calc'd for C13H18N5[M+H]+, 244; found 244. 1H NMR (500 MHz, DMSO-D6) δ 12.7 (br s, 1H), 9.21 (br s, 2H), 8.35 (s, 1H), 7.47 (s, 1H), 6.85 (s, 1H), 4.56 (br s, 1H), 4.30-3.76 (br m, 4H), 3.20-3.02 (br m, 2H), 2.60 (br pentet, 1H), 2.33-2.24 (br m, 1H), 2.22-2.14 (br m, 1H), 1.82-1.74 (br m, 1H), 1,74-1.52 (br m, 2H).

Provenance & Evidence