Fumaric Acid → HCID 131711122, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 1-(1-methyl-1H-tetrazol-5-yl)aminomethyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline dihydrochloride (52.3 g) and water (300 ml) was stirred for 15 minutes at 100° C to give homogeneous solution. Fumaric acid (11.3 g) was added thereto at 100° C, to which was added water (50 ml). The mixture was stirred for 15 minutes, to which were added sodium bicarbonate (25.2 g) over 12 minutes and water (50 ml). The resultant mixture was stirred for 20 minutes at 100° C and the reaction mixture was filtered. The filtrate was allowed to stand at ambient temperature to precipitate crystals. The crystals were collected by filtration, washed with water and dried under reduced pressure to give 1-(1-methyl-1H-tetrazol-5-yl)aminomethyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hemifumarate (42.05 g), mp 204° to 207° C (dec.).

Provenance & Evidence