Hydrochloric Acid → HCID 13457907, compound

Participants

Reaction Steps

To a stirred solution of cis-1,3,4,6,7,11b-hexahydro-7-phenyl-2H-pyrazino[2,1-a]isoquinoline dihydrochloride (7.8 g, 0.023 m) and triethylamine (9.4 g, 0.93 m) in chloroform (100 ml) maintained at 0° under nitrogen was added dropwise butyryl chloride (3.8 g, 0.0356 m). The mixture was allowed to warm to ambient temperature and stirred for 3 hours, then treated with 10% HCl (50 ml). The layers were separated and the organic phase washed with 10% HCl (2×50 ml), water (50 ml), and dried over MgSO4. Evaporation of the solvent gave an oily residue which was dissolved in tetrahydrofuran (100 ml) and a white solid crystallized which was collected by filtration to give 5.1 g of cis-1,3,4,6,7,11b-hexahydro-2-butyryl-7-phenyl-2H-pyrazino[2,1-a]isoquinoline, m.p. 212°-213°. An additional 3.5 of good purity product was recovered from the tetrahydrofuran to give a total of 8.6 g (93%).

Provenance & Evidence