HCID 140370881, compound → HCID 140370878, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 44 (20 g, 0.07 mol) in 200 mL of 30-32% HBr in acetic acid was vigorously stirred along with gradual heating (temperature up to 120° C.) over a period of 1 h. The mixture was cooled and filtered. The colorless crystals were washed with acetic acid (200 mL), ether (200 mL) and dried in vacuo overnight to give 22.6 g (80%) of 45: mp 170°-172° C. (dec) (note: Incomplete reaction will occur if the stirring is not efficient); 1H NMR (DMSO-d6) δ 3.05 [t, 2, --CH2 --C(N=)], 3.5 (b, 4, --CH2 --NH--CH2), 3.78, (t, 2, BrCH2 --).

Provenance & Evidence