Hydrochloric Acid → HCID 13457904, compound

Participants

Reaction Steps

To a stirred solution of 1.0 M borane in tetrahydrofuran (55 ml) maintained under nitrogen at 0° C. was added cis-1,3,4,6,7,11b-hexahydro-7-phenyl-2-propionyl-2H-pyrazino[ 2,1-a]isoquinoline (5.3 g, 0.016 m) and the mixture heated to reflux for 3 hours, then cooled in an ice bath and carefully treated with 10% HCl (100 ml). This mixture was heated to reflux for 1 hour, then cooled, and the tetrahydrofuran removed on an aspirator. The remaining aqueous solution was basified to pH 11 with 50% NaOH and extracted with chloroform. The extracts were dried over MgSO4 and evaporated to a solid residue (6.0 g). This was dissolved in methanol (50 ml) and isopropanol (50 ml) and acidified with HCl gas. Upon cooling and standing, a white solid crystallized, which was collected by filtration and vacuum dried at 80° for 24 hours to give 4.6 g cis-1,3,4,6,7,11b-hexahydro-7-phenyl-2-propyl-2H-pyrazino[2,1-a]isoquinoline dihydrochloride, m.p. 273°-274°.

Provenance & Evidence