Fumaric Acid → HCID 19095345, compound

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Reaction Steps

3,4-Dihydro-1-methyl-6-[4-(trifluoromethyl)-phenyl]pyrrolo[1,2-a]pyrazine (2.5 g) was dissolved in a mixture of 130 ml of methanol and 13 ml of water under argon. The solution was treated portionwise with 1.0 g of sodium borohydride while stirring and stirred at room temperature overnight. Thereafter, the methanol was removed in a vacuum, the residue was taken up in 100 ml of methylene chloride and washed with 80 ml of 10% ammonia solution. The phases were separated and the aqueous phase was extracted twice with 50 ml of methylene chloride each time. The organic phases were combined, dried with MgSO4 and freed from solvent. The crude product, 2.5 g of yellow-brown solid, was dissolved in a 20-fold amount of ethanol, treated with 1.1 equivalents of a saturated solution of fumaric acid in ethanol and concentrated to 40 ml. There were obtained 2.5 g (70%) of 1,2,3,4-tetrahydro-1-methyl-6-[4-(trifluoromethyl)phenyl]pyrrolo[1,2-a]pyrazine fumarate (1:1); m.pt.: 180°-183° C. (dec.).

Provenance & Evidence