Phosphoric Acid → HCID 67237812, compound

Participants

Reaction Steps

To a solution of 6.70 g (0.0273 mol) (3R,5R,8aR)-3,5-Dimethyl-1,3,5,6,7,8,8a,9-octahydro-2-oxa-4,4b,7-triaza-cyclopenta[b]fluorene in 90 ml methanol was added a solution of 2.67 g (0.0273 mol) ortho phosphoric acid in 30 ml methanol and the mixture was stirred at room temperature for 1 h. The solvent was evaporated and the residue was taken up in 130 ml ethanol. To the mixture were added seed crystals and stirring was continued for 22 h. The solids were collected by filtration and dried to constant weight under high vacuum to yield 8.74 g (3R,5R,8aR)-3,5-dimethyl-1,3,5,6,7,8,8a,9-octahydro-2-oxa-4,4b,7-triaza-cyclopenta[b]fluorene dihydrogenphosphate as white crystals. (elemental analysis calculated C, 48.83H, 6.47 N, 12.20 found C, 48.77H, 6.38 N, 12.08)

Provenance & Evidence