Acetic Acid → HCID 14620595、化合物

反応式

Br.C(O)(=O)C.C[O:7][C:8]1[C:9]([O:27]C)=[CH:10][C:11]2[CH2:12][CH2:13][N:14]3[CH2:20][CH2:19][C:18]4[CH:21]=[CH:22][CH:23]=[CH:24][C:17]=4[CH2:16][CH:15]3[C:25]=2[CH:26]=1>O1CCCC1>[CH:26]1[C:25]2[CH:15]3[CH2:16][C:17]4[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=4[CH2:19][CH2:20][N:14]3[CH2:13][CH2:12][C:11]=2[CH:10]=[C:9]([OH:27])[C:8]=1[OH:7]

参加物

実験手順

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°.