Sulfuric Acid → N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide sulfate

Participants

Reaction Steps

To a solution of N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (1.10 g) in acetone (150 ml) was added at room temperature 47% sulfuric acid (0.27 ml), and the mixture was stirred for 0.5 hours and concentrated under reduced pressure. To the residue was added 2-propanol, and the mixture was concentrated. To the residue was added 2-propanol, and the resulting solid was collected by filtration and dissolved in 2-propanol under heating. The solution was cooled, and the resulting powder was collected by filtration to give colorless amorphous of N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide sulfate (Compound 148) (1.21 g).

Provenance & Evidence