Hydrogen Bromide → HCID 178419258, compound

Participants

Reaction Steps

Compound 19 (10 g, 0.048 mol) was added in portions to a well stirred saturated solution of 100 mL of HBr in AcOH at room temperature. After addition, the mixture was stirred overnight, the precipitated solid was separated by filtration, washed with ether (200 mL) and dried in vacuo over KOH. Recrystallization from methanol-ether afforded 14.2 g (80%) of 20 as colorless crystals: mp 155° C. (dec); 1H NMR (CD3OD) δ 2.96 (s, 3, NCH3), 3.05 [t, 2, CH2CH2 (NH)], 3.49-3.64 (m, 4, CH2N--CH2) and 3.8 (t, 2, CH2CH2Br).

Provenance & Evidence