Acetic Acid → HCID 14620595, compound

Participants

Reaction Steps

Hydrobromic acid (48%, 30 ml) was added to a glacial acetic acid (3 ml) solution of 5,6,8,9,14,14a-hexahydro-2,3-dimethoxyisoquino[1,2-b][3]-benzazepine (XIIIc, Ex. 20) (0.928 g, 3 mmole), and the resulting solution was heated under reflux for 2.5 hours, then evaporated on a rotary evaporator to give a resinous residue. The residue was dissolved in tetrahydrofurane (about 80 ml), and the solution was allowed to sit at room temperature over a weekend. The crystalline product that was separated was collected on a filter, and washed with tetrahydrofurane to give the titled product which was recrystallized from ethanol. The product (HBr salt) weighed 0.8 g (73%) and melted at 270°-272°.

Provenance & Evidence