Benzenesulfonic 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 benzenesulfonate

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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 THF (40 ml) was added at room temperature benzenesulfonic acid (313 mg), and the mixture was stirred for 1 hour and concentrated under reduced pressure. To the residue was added 2-propanol, and the mixture was concentrated under reduced pressure. The residue was crystallized from 2-propanol to give crude crystals, which were recrystallized 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 benzenesulfonate (Compound 147) (1.19 g).

Provenance & Evidence