Methanesulfonic 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 methanesulfonate

Participants

Reaction Steps

To a suspension 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 (0.80 g) in ethanol (50 ml) was added at room temperature methanesulfonic acid (84 μl), and the mixture was stirred for 1 hour and concentrated under reduced pressure. The residue was crystallized from 2-propanol to give colorless crystals 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 methanesulfonate (Compound 146) (0.78 g).

Provenance & Evidence